CN115138105B - Novel polymer defoamer for waterproof paint and preparation method thereof - Google Patents
Novel polymer defoamer for waterproof paint and preparation method thereof Download PDFInfo
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- CN115138105B CN115138105B CN202210927734.9A CN202210927734A CN115138105B CN 115138105 B CN115138105 B CN 115138105B CN 202210927734 A CN202210927734 A CN 202210927734A CN 115138105 B CN115138105 B CN 115138105B
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- heptamethyltrisiloxane
- polymer defoamer
- oleic acid
- novel polymer
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- 239000013530 defoamer Substances 0.000 title claims abstract description 37
- 229920000642 polymer Polymers 0.000 title claims abstract description 31
- 239000003973 paint Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- SWGZAKPJNWCPRY-UHFFFAOYSA-N methyl-bis(trimethylsilyloxy)silicon Chemical compound C[Si](C)(C)O[Si](C)O[Si](C)(C)C SWGZAKPJNWCPRY-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 24
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 24
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 23
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 23
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 23
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000005642 Oleic acid Substances 0.000 claims abstract description 23
- -1 amino carbon nanotubes Chemical compound 0.000 claims abstract description 23
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 23
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 23
- 239000003054 catalyst Substances 0.000 claims abstract description 18
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 17
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 22
- 229920001289 polyvinyl ether Polymers 0.000 claims description 6
- 239000000376 reactant Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 239000006260 foam Substances 0.000 abstract description 10
- 230000002401 inhibitory effect Effects 0.000 abstract description 3
- 239000004721 Polyphenylene oxide Substances 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 9
- 238000000576 coating method Methods 0.000 description 9
- 229920000570 polyether Polymers 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 239000002518 antifoaming agent Substances 0.000 description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000010276 construction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000003995 emulsifying agent Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000007112 amidation reaction Methods 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
- B01D19/0404—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
- B01D19/0404—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
- B01D19/0409—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance compounds containing Si-atoms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
- B01D19/0404—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
- B01D19/0413—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance compounds containing N-atoms
Abstract
The invention discloses a novel polymer defoamer for waterproof paint and a preparation method thereof, wherein the novel polymer defoamer is composed of 5-20 parts of oleic acid polyoxyethylene ether, 5-15 parts of amino carbon nanotubes, 10-40 parts of heptamethyltrisiloxane and 0.5-1 part of bimetallic catalyst DMC. Firstly, enabling oleic acid polyoxyethylene ether to react with an amino carbon nano tube, then adding a bimetallic catalyst DMC, and finally adding heptamethyltrisiloxane in batches for reaction, thereby obtaining the novel polymer defoamer. The novel polymer defoamer prepared by the invention can obviously improve defoaming and foam inhibiting capabilities.
Description
Technical Field
The invention relates to the field of defoamers, in particular to a novel polymer defoamer for waterproof paint and a preparation method thereof.
Background
The waterproof coating is widely applied in building decoration industry, such as house building, outer wall, indoor, urban road, tunnel, subway reservoir and the like. The waterproof coating material forms a coating film capable of preventing rainwater and underground infiltration, but the appearance of foam also has an effect on the performance of the waterproof coating material.
If the waterproof coating is foamed in the production process, the volume expansion of the surfactant is caused in the process of compatible stirring, and the utilization rate of blending equipment is reduced; the foam limits the stirring speed, so that the blending time of the waterproof paint is prolonged, and the filler and the dye cannot be fully wetted; if the foam is durable, the construction process can be influenced, so that the fluidity of the construction process is poor, and the conditions of surface defects, roughness, rupture during film formation and the like appear.
The waterproof paint defoamers used at present are various, but the defoamers have poor defoaming and foam inhibition and dilute and drift oil, when in use, after the emulsifier is separated from the surface of the defoamer due to certain reasons (such as water is added for dilution before coating), the water-insoluble defoamer is easy to cause shrinkage cavity and fish eye phenomena on the surface of a coating film.
Disclosure of Invention
The invention aims to provide a novel polymer defoamer for waterproof paint and a preparation method thereof, which are used for solving the problem of poor defoaming and foam inhibiting capability of the defoamer for the waterproof paint in the prior art.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the novel polymer defoamer for the waterproof paint comprises the following components in parts by weight:
5-20 parts of oleic acid polyoxyethylene ether,
5-15 Parts of amino carbon nano tube,
10-40 Parts of heptamethyltrisiloxane,
0.5-1 Part of bimetallic catalyst DMC.
Further, the components in parts by weight are as follows:
10 parts of oleic acid polyoxyethylene ether,
15 Parts of amino carbon nano-tube,
20 Parts of heptamethyltrisiloxane,
0.5 Part of bimetallic catalyst DMC.
A method for preparing a novel polymer defoamer, comprising the following steps:
and step 1, weighing and mixing the oleic acid polyvinyl ether and the amino carbon nanotubes according to parts by weight, and stirring and reacting the mixture of the oleic acid polyvinyl ether and the amino carbon nanotubes for 1.8-3.5 hours at the temperature of 70-90 ℃ to obtain an intermediate reactant. In this step 1, the carboxyl end group of the oleic acid polyvinyl ether and the amino group of the amino carbon nanotube can be allowed to sufficiently contact and react, thereby introducing the carbon nanotube into the oleic acid polyvinyl ether.
And 2, weighing the bimetallic catalyst DMC and the heptamethyltrisiloxane according to parts by weight, adding the weighed bimetallic catalyst into the intermediate reactant obtained in the step 1, adding the heptamethyltrisiloxane in batches, and stirring and reacting for 1.7-2.2 hours at the temperature of 60-80 ℃ to obtain the novel polymer defoamer.
In the step 1, the stirring speed is 800-1000 r/min.
Further, in the step 1, the mixture of the two is stirred and reacted for 3 hours at the temperature of 80 ℃ to obtain an intermediate reactant.
In the step 2, the stirring speed is 1200-1500 r/min.
Further, in the step 2, the addition is completed by adopting a mode of dropwise adding heptamethyltrisiloxane and controlling for 30 minutes,
Further, in the step 2, stirring and reacting for 2 hours at the temperature of 70 ℃ to obtain the novel polymer defoamer.
The principle of the invention is as follows:
The invention adopts oleic acid polyoxyethylene ether as one of the raw materials, and the oleic acid polyoxyethylene ether is carboxyl end capped polyether. Polyether itself has good defoaming property as a defoaming agent, but is greatly affected by temperature, and when the temperature is increased or changed greatly, the defoaming effect is greatly impaired. The oleic acid polyoxyethylene ether selected by the invention has carboxyl groups with higher activity, and is easier to react with other groups for modification, so that the defect is overcome; and the emulsion has good emulsifying property, does not need to additionally add an emulsifying agent, and reduces the production cost.
The invention adopts amino carbon nano tube as one of the raw materials. The amino carbon nanotube is a substance with extremely high length-diameter ratio, molecules are rod-shaped, formed foam can be broken, and good foam breaking effect is achieved.
The invention adopts heptamethyltrisiloxane as one of the raw materials. The molecular structure of heptamethyltrisiloxane is as follows:
The heptamethyltrisiloxane has a series of advantages of low surface tension, small viscosity-temperature coefficient, high and low temperature resistance, oxidation resistance stability, weather resistance, corrosion resistance and the like, and the use of the heptamethyltrisiloxane modified polyether can obviously improve the defoaming capability and stability of the system; the methyl has extremely low surface tension, and the quantity of the methyl heptamethyltrisiloxane selected by the invention is large, so that the surface tension of a defoaming system can be obviously reduced, and the defoaming effect is achieved.
Therefore, compared with the prior art, the novel polymer defoamer prepared by the invention can obviously improve defoaming and foam inhibiting capability and has the advantages of low cost, good tolerance and stability.
Detailed Description
The invention is further illustrated below with reference to examples.
Example 1
The novel polymer defoamer for waterproof paint of the embodiment 1 comprises the following components in parts by weight:
10 parts of oleic acid polyoxyethylene ether,
10 Parts of amino carbon nano-tube,
10 Parts of heptamethyltrisiloxane,
0.5 Part of bimetallic catalyst DMC.
The preparation method of the novel polymer defoamer in the embodiment 1 comprises the following steps:
step 1, placing 10 parts of oleic acid polyoxyethylene ether and 10 parts of amino carbon nanotubes in a three-neck flask with a thermometer, stirring at 80 ℃ and a rotating speed of 800-1000r/min, and continuously reacting for 3 hours.
And 2, putting the prepared polyether into a three-neck flask with a thermometer, firstly adding 0.5 part of a bimetallic catalyst DMC, controlling the dropwise addition of heptamethyltrisiloxane for 30 minutes, and finally continuously stirring at the temperature of 70 ℃ for 2 hours at the rotating speed of 1200-1500r/min to enable the reaction to be carried out, thus obtaining the novel polymer defoamer A.
Example 2
The novel polymer defoamer for waterproof paint of the embodiment 2 comprises the following components in parts by weight:
10 parts of oleic acid polyoxyethylene ether,
15 Parts of amino carbon nano-tube,
10 Parts of heptamethyltrisiloxane,
0.5 Part of bimetallic catalyst DMC.
The preparation method of the novel polymer defoamer in the embodiment 2 comprises the following steps:
Step 1, placing 10 parts of oleic acid polyoxyethylene ether and15 parts of amino carbon nanotubes in a three-neck flask with a thermometer, stirring at 80 ℃ and a rotating speed of 800-1000r/min, and continuously reacting for 3 hours.
And 2, putting the prepared polyether into a three-neck flask with a thermometer, firstly adding 0.5 part of a bimetallic catalyst DMC, controlling the dropwise addition of heptamethyltrisiloxane for 30 minutes, and finally continuously stirring at the temperature of 70 ℃ for 2 hours at the rotating speed of 1200-1500r/min to enable the reaction to be carried out, thus obtaining the novel polymer defoamer B.
Example 3
The novel polymer defoamer for waterproof paint of the embodiment 3 comprises the following components in parts by weight:
10 parts of oleic acid polyoxyethylene ether,
10 Parts of amino carbon nano-tube,
20 Parts of heptamethyltrisiloxane,
0.5 Part of bimetallic catalyst DMC.
The preparation method of the novel polymer defoamer in the embodiment 3 comprises the following steps:
step 1, placing 10 parts of oleic acid polyoxyethylene ether and 10 parts of amino carbon nanotubes in a three-neck flask with a thermometer, stirring at 80 ℃ and a rotating speed of 800-1000r/min, and continuously reacting for 3 hours.
Step 2, putting the prepared polyether into a three-neck flask with a thermometer, firstly adding 0.5 part of a bimetallic catalyst DMC, dropwise adding heptamethyltrisiloxane, controlling the dropwise adding time to be 30 minutes, and finally continuously stirring at the temperature of 70 ℃ for 2 hours at the rotating speed of 1200-1500r/min to enable the reaction to be carried out, thus obtaining the novel polymer defoamer C.
Example 4
The novel polymer defoamer for waterproof paint of the embodiment 4 comprises the following components in parts by weight:
10 parts of oleic acid polyoxyethylene ether,
15 Parts of amino carbon nano-tube,
20 Parts of heptamethyltrisiloxane,
0.5 Part of bimetallic catalyst DMC.
The preparation method of the novel polymer defoamer of the embodiment 4 comprises the following steps:
Step 1, placing 10 parts of oleic acid polyoxyethylene ether and15 parts of amino carbon nanotubes in a three-neck flask with a thermometer, stirring at 80 ℃ and a rotating speed of 800-1000r/min, and continuously reacting for 3 hours.
And 2, putting the prepared polyether into a three-neck flask with a thermometer, firstly adding 0.5 part of a bimetallic catalyst DMC, adopting a mode of dropwise adding heptamethyltrisiloxane, controlling the addition to be completed for 30 minutes, and finally continuously stirring at the temperature of 70 ℃ for 2 hours at the rotating speed of 1200-1500r/min to enable the reaction to be carried out, thus obtaining the novel polymer defoamer D.
The performance experiments of the novel polymeric defoamers A, B, C, D prepared in examples 1-4, respectively, were as follows:
(1) 40mL of waterproof paint is placed in a measuring cylinder with a plug (the upper scale of the measuring cylinder extends to be calibrated to 140mL, and the lower scale extends to be 5 mL), and 0.02mL of defoaming agent is added. The solution was vigorously shaken 30 times at a rate of 2 times/s and the foam maximum height H 0 was recorded. Each group of solutions was measured 5 times and averaged.
The defoamer prepared by the invention is compared with the defoamer for the common waterproof coating on the market, and the results are shown in table 1:
Table 1 comparison results table
Defoaming agent | Example 1A | Example 2 is B | Example 3 is C | Example 4 is D | Ⅰ | Ⅱ | Blank space |
H0/ml | 79 | 75 | 74 | 71 | 75 | 78 | 85 |
In Table 1, I, II are representative different comparisons used by market clients, respectively.
Comparing the two groups of experiments 1 and 2, it can be seen that when the mass ratio of carboxyl-terminated polyether to amino carbon nano tube is 4:3, the higher the amidation reaction degree, the better the defoaming effect. As can be seen from comparing the two groups of experimental results 1 and 3, the defoaming effect is improved along with the increase of the content of the heptamethyltrisiloxane in the reaction. Throughout the experiments, the novel polymeric defoamer D obtained in example 4 has the most remarkable effect, so that when carboxyl terminated polyether: amino carbon nanotubes=4:3, with appropriate increase of heptamethyltrisiloxane content, being the best choice.
(2) And (3) respectively putting the defoaming agents for the paint into 6 barrels of the same paint, uniformly stirring, and then coating the paint on the same wall surface with the number of 1-6 for experiments. The test shows that the number of the small bubbles on the No. 1-4 wall surface is less than that of the paint without the defoaming agent for the paint. In particular, the novel polymer defoamer D of example 4 produced a minimum number of small bubbles.
The embodiments of the present invention are merely described in terms of preferred embodiments of the present invention, and are not intended to limit the spirit and scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope of the present invention, and the technical content of the present invention as claimed is fully described in the claims.
Claims (3)
1. The polymer defoamer for the waterproof paint is characterized by comprising the following components in parts by weight:
5-20 parts of oleic acid polyoxyethylene ether,
5-15 Parts of amino carbon nano tube,
10-40 Parts of heptamethyltrisiloxane,
0.5-1 Part of bimetallic catalyst DMC;
the preparation method comprises the following steps:
Step 1, weighing and mixing oleic acid polyvinyl ether and amino carbon nanotubes according to parts by weight, and mixing the oleic acid polyvinyl ether and the amino carbon nanotubes at 70-90 DEG C
Stirring and reacting for 1.8-3.5 hours under the condition to obtain an intermediate reactant; and 2, weighing the bimetallic catalyst DMC and the heptamethyltrisiloxane according to parts by weight, adding the weighed bimetallic catalyst into the intermediate reactant obtained in the step1, then adding the heptamethyltrisiloxane in batches, and stirring and reacting for 1.7-2.2 hours at the temperature of 60-80 ℃ to obtain the polymer defoamer.
2. The polymer defoamer for waterproof paint of claim 1, wherein the components are as follows in parts by weight:
10 parts of oleic acid polyoxyethylene ether,
15 Parts of amino carbon nano-tube,
20 Parts of heptamethyltrisiloxane,
0.5 Part of bimetallic catalyst DMC.
3. The polymer defoamer for waterproof paint according to claim 1, which is prepared by the following steps:
In the step 1, stirring speed is 800-1000 r/min, and stirring and reacting a mixture of the two at 80 ℃ for 3 hours to obtain an intermediate reactant;
in the step 2, the stirring speed is 1200-1500 r/min, heptamethyltrisiloxane is added dropwise for 30 minutes, and the polymer defoamer is obtained after stirring reaction for 2 hours at 70 ℃.
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