CN110818890A - Super-spreading wetting agent and preparation method thereof - Google Patents

Super-spreading wetting agent and preparation method thereof Download PDF

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CN110818890A
CN110818890A CN201911158548.8A CN201911158548A CN110818890A CN 110818890 A CN110818890 A CN 110818890A CN 201911158548 A CN201911158548 A CN 201911158548A CN 110818890 A CN110818890 A CN 110818890A
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wetting agent
alkynediol
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邱元进
饶长贵
陈国栋
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Fujian Huaxialan New Material Technology Co Ltd
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Abstract

The invention discloses a super-spreading wetting agent which is silane modified alkynediol polyether. The supercritical micelle concentration of the super-spreading wetting agent in water is low, and the super-spreading wetting agent shows a super-spreading phenomenon on the surface of a base material and has an excellent wetting effect on the base material; the super-spreading wetting agent has short balancing time in an aqueous system and larger difference of the internal and external surface tension of bubbles, counteracts Gibbs-Marangoni effect, enables the bubbles to break rapidly and is an unstable-foaming surfactant.

Description

Super-spreading wetting agent and preparation method thereof
Technical Field
The invention relates to a super-spreading wetting agent and a preparation method thereof.
Background
With the development of science and technology and the improvement of environmental protection requirements of people, water-based adhesives and water-based coatings move to the stage and gradually replace solvent-based adhesives and coatings. The water-based adhesive and the water-based paint both use water as a dispersion medium, so that a large amount of solvents which harm human bodies and the environment are avoided, social resources are saved, and contribution to sustainable development is made. Due to the high surface tension of water (72 mN/m), it is difficult to wet most substrates. In practice, one often adds a wetting agent to facilitate wetting of the substrate by the system. Wetting agents are a class of surfactants that can make solid materials more wettable by water or other liquids by lowering the surface energy. With a certain amount of wetting agent, it is desirable that the aqueous system achieve complete spreading and wetting, i.e., superspreading, on the substrate surface. Therefore, the super-spreading requires that the concentration of the super-spreading liquid in the system is far from the supercritical micelle concentration (CMC), which puts high requirements on a wetting agent.
Among the wetting agents commonly found on the market are small molecule wetting agents (e.g. cyanohydrin)®OT-75), modified polyether wetting agents (e.g., Dow chemical Triton)®X-405 and Ecosurf®BD-405, etc.), silicone wetting agents (e.g., digavin)®4100 and Wet®270, etc.) and acetylenic diol wetting agents (e.g., Surfynol, U.S. air chemistry)®104E) And the like.
The micromolecule wetting agent, the modified polyether wetting agent and the organic silicon wetting agent have good wetting effect on the base material, and the organic silicon wetting agent is especially due to extremely low surface tension, so that certain optimized structures can achieve the super-spreading effect; but the foam is more due to disturbance and dispersion during use, etc., which may affect the properties of the final product. The electron-withdrawing structure characteristic of the alkynyl of the alkynediol wetting agent determines that the foaming property is low, but on one hand, the surface tension of the alkynyl of a hydrophobic group in the alkynediol is high (about 30 mN/m), on the other hand, the hydrophilic group accounts for a relatively high proportion, the compatibility with an aqueous system is too good, and the Critical Micelle Concentration (CMC) in the system is relatively high, so that the use amount of the alkynediol wetting agent is difficult to achieve the superspreading effect in practical application.
Disclosure of Invention
The invention aims to provide a super-spreading wetting agent and a preparation method thereof. The technical scheme adopted by the invention is that the superspreading wetting agent has a structural general formula as follows:
wherein R is1And R2Are respectively one of hydrogen, methyl and n-butyl, and R1And R2Not hydrogen at the same time;
R3and R4Are respectively as
Figure 169271DEST_PATH_IMAGE002
C is an integer of 0-15, d is an integer of 0-6, and c + d is more than or equal to 2 and less than or equal to 15;
R5is one of methylene and trimethylene;
the preparation method of the super-spreading wetting agent comprises the following steps:
(1) adding 0.001-0.006 mol of catalyst into 1 mol of alkynyl compound subjected to molecular sieve dehydration under the protection of nitrogen, introducing 4-30 mol of polymerization monomer, heating to 90-120 ℃, keeping the temperature for 3-9 hours, and cooling to 30-40 ℃; introducing the reaction product into a mixed bed type ion exchange column activated by ethanol to remove the catalyst, and obtaining alkynediol polyether;
(2) adding an alcohol solution containing 2 mol of alkali metal alcoholate into alkynediol polyether, heating to 65-80 ℃, keeping a slight boiling state, slowly distilling out alcohol, keeping for 2-6 hours, and then distilling under reduced pressure to remove the alcohol; cooling to 25-35 ℃ to obtain alkali metal salt of the alkynediol polyether;
(3) dripping 2.2-2.8 mol of chlorinating agent into 2 mol of organic silicon compound within 0.5-2 hours, stirring for 2-4 hours at 0-30 ℃, and removing the redundant chlorinating agent by vacuum filtration to obtain the chloride of the organic silicon compound;
(4) and (3) adding the chloride of the silicon compound obtained in the step (3) into the alkali metal salt of the alkynediol polyether obtained in the step (2), reacting for 2-5 hours at 25-40 ℃, and filtering to remove generated solid salt to obtain the super-spreading wetting agent.
Wherein the alkynyl compound is one of 3-hexyne-2, 5-diol, 2, 5-dimethyl-3-hexyne-2, 5-diol and 5, 8-dimethyl-6-dodecyne-5, 8-diol;
the catalyst is one of zinc hexacyanocobaltate, potassium hydroxide and lithium hydroxide;
the polymerized monomer is one or a combination of two of ethylene oxide and propylene oxide;
the alkali metal alcoholate is one or a combination of sodium methoxide, potassium methoxide, sodium ethoxide and potassium ethoxide;
the organic silicon compound is one of 3- (3-hydroxymethyl) heptamethyltrisiloxane and 3- (3-hydroxypropyl) heptamethyltrisiloxane;
the chlorinating agent is one of thionyl chloride and sulfuryl chloride.
Compared with the prior art, the superspreading wetting agent is silane modified alkyne diol polyether, the alkyne diol polyether is a surfactant with better compatibility with various systems, the static surface tension of the surfactant is 30-35 mN/m, the dynamic surface tension of the surfactant is about 35-41 mN/m, and the surfactant has good wetting effect on various base materials; after the modification by the heptamethyltrisilane compound, the static surface tension can be further reduced to be close to that of organic silicon (21-25 mN/m), and the dynamic surface tension is reduced to 28-36 mN/m; due to the existence of silicon base, the solubility of the super-spreading wetting agent in water is reduced, the critical micelle concentration of the super-spreading wetting agent in water is reduced, and the super-spreading effect is shown on the surface of the substrate; meanwhile, the overspread wetting agent foam is lower than other kinds of wetting agent foams due to the smaller difference between the dynamic surface tension and the static surface tension.
The super spreading wetting agent is silane modified alkynediol polyether. The alkynyl in the alkynediol polyether and the adjacent alkyl form a linear hydrophobic structure with strong rigidity, so that compact rigid ordered arrangement is easily formed on the liquid surface quickly, the surface tension of the liquid is reduced, and the foam is strongly damaged; after the modification by the heptamethyltrisilane compound, the static surface tension can be further reduced to be close to (21-25 mN/m) of an organosilicon wetting agent, and the dynamic surface tension is reduced to 28-36 mN/m; due to the existence of silicon base, the solubility of the super-spreading wetting agent in water is reduced, the critical micelle concentration of the super-spreading wetting agent in water is reduced, and the super-spreading effect is shown on the surface of the substrate; meanwhile, the super-spreading wetting agent has low dynamic surface tension, short balancing time in an aqueous system and large difference of the internal and external surface tension of the bubbles, so that the Gibbs-Marangoni effect is counteracted, the bubbles are rapidly broken, and the super-spreading wetting agent is an unstable-foaming surfactant.
Detailed Description
The present invention is further illustrated by the following examples.
Example 1
The preparation method of the super-spreading wetting agent comprises the following steps:
(1) adding 0.001 mol of catalyst lithium hydroxide into 1 mol of 5, 8-dimethyl-6-dodecyne-5, 8-diol dehydrated by a molecular sieve under the protection of nitrogen, introducing 8 mol of ethylene oxide, heating to 90 ℃, keeping the temperature for 3 hours, and cooling to 40 ℃; introducing the reaction product into an ethanol activated mixed bed type ion exchange column to remove the catalyst, and obtaining acetylene glycol polyoxyethylene ether-0400;
(2) adding a methanol solution containing 2 mol of potassium methoxide into acetylene glycol polyoxyethylene ether-0400, heating to 65 ℃, keeping the temperature slightly boiling, slowly distilling out methanol, keeping for 2 hours, and then distilling under reduced pressure to remove residual methanol; cooling to 25 ℃ to obtain sylvite of alkynediol polyoxyethylene ether-0400;
(3) dropwise adding 2.2 mol of sulfonyl chloride into 2 mol of 3- (3-hydroxypropyl) heptamethyltrisiloxane within 2 hours, stirring for 4 hours at 10 ℃, and removing redundant sulfonyl chloride by vacuum filtration to obtain 3- (3-chloropropyl) heptamethyltrisiloxane;
(4) slowly adding 3- (3-chloropropyl) heptamethyltrisiloxane into acetylene glycol polyoxyethylene ether-0400 potassium salt, reacting for 2 hours at 40 ℃, and filtering to remove generated potassium chloride to obtain the super-spreading wetting agent W1.
Example 2
The preparation method of the super-spreading wetting agent comprises the following steps:
(1) adding 0.004 mol of catalyst potassium hydroxide into 1 mol of 3-hexyne-2, 5-diol dehydrated by a molecular sieve under the protection of nitrogen, introducing 12 mol of propylene oxide, heating to 115 ℃, keeping the temperature for 7 hours, and cooling to 35 ℃; introducing the reaction product into a mixed bed type ion exchange column activated by ethanol to remove the catalyst, and obtaining the alkynediol polyoxypropylene ether-0006;
(2) adding an ethanol solution containing 2 mol of sodium ethoxide into alkynediol polyoxypropylene ether-0006, heating to 80 ℃, keeping the temperature slightly boiling, slowly distilling out ethanol, keeping for 4 hours, and then distilling under reduced pressure to remove residual ethanol; cooling to 25 ℃ to obtain alkynediol polyoxypropylene ether-0006 sodium salt;
(3) dropwise adding 2.8 mol of thionyl chloride into 2 mol of 3- (3-hydroxymethyl) heptamethyltrisiloxane within 0.5 hour, stirring for 2 hours at 30 ℃, and carrying out vacuum filtration to remove excessive thionyl chloride to obtain 3- (3-chloromethyl) heptamethyltrisiloxane;
(4) adding 3- (3-chloromethyl) heptamethyltrisiloxane into alkynediol polyoxypropylene ether-0006 sodium salt, reacting for 5 hours at 25 ℃, and filtering to remove generated sodium chloride to obtain the super-spreading wetting agent W2.
Example 3
The preparation method of the super-spreading wetting agent comprises the following steps:
(1) adding 0.005mol of catalyst zinc hexacyanocobaltate into 1 mol of 2, 5-dimethyl-3-hexyne-2, 5-diol dehydrated by a molecular sieve under the protection of nitrogen, introducing 22 mol of ethylene oxide and 8 mol of propylene oxide, heating to 120 ℃, keeping the temperature for 9 hours, and cooling to 35 ℃; introducing the reaction product into a mixed bed type ion exchange column activated by ethanol to remove the catalyst, and obtaining alkynediol polyoxyethylene polyoxypropylene ether-1104;
(2) adding an ethanol solution containing 1 mol of potassium ethoxide and an ethanol solution containing 1 mol of potassium methoxide into alkynediol polyoxyethylene polyoxypropylene ether-1104, heating to 65 ℃, keeping the mixture in a slightly boiling state for 2 hours, slowly distilling out methanol, heating to 78 ℃ after the methanol is basically distilled out, slowly distilling out the ethanol, keeping for 4 hours, and distilling under reduced pressure to remove residual ethanol; cooling to 30 ℃ to obtain sylvite of alkynediol polyoxyethylene polyoxypropylene ether-1104;
(3) dropwise adding 2.5 mol of thionyl chloride into 2 mol of 3- (3-hydroxypropyl) heptamethyltrisiloxane within 1 hour, stirring for 2.5 hours at 0 ℃, and carrying out vacuum filtration to remove redundant thionyl chloride to obtain 3- (3-chloropropyl) heptamethyltrisiloxane;
(4) adding 3- (3-chloropropyl) heptamethyltrisiloxane into alkynediol polyoxyethylene polyoxypropylene ether-1104 potassium salt, reacting for 4 hours at 30 ℃, and filtering to remove generated potassium chloride to obtain the super-spreading wetting agent W3.
Example 4
The preparation method of the super-spreading wetting agent comprises the following steps:
(1) adding 0.002 mol of catalyst lithium hydroxide into 1 mol of 5, 8-dimethyl-6-dodecyne-5, 8-diol dehydrated by a molecular sieve under the protection of nitrogen, introducing 30 mol of ethylene oxide, heating to 105 ℃, keeping the temperature for 9 hours, and cooling to 30 ℃; introducing the reaction product into a mixed bed type ion exchange column activated by ethanol to remove the catalyst, and obtaining alkynediol polyoxyethylene ether-1500;
(2) adding a methanol solution containing 2 mol of sodium methoxide into alkynediol polyoxyethylene ether-1500, heating to 65 ℃, keeping the temperature slightly boiling, slowly distilling out methanol, keeping for 3 hours, and then distilling under reduced pressure to remove residual methanol; cooling to 35 ℃ to obtain alkynediol polyoxyethylene ether-1500 sodium salt;
(3) dropwise adding 2.3 mol of sulfonyl chloride into 2 mol of 3- (3-hydroxymethyl) heptamethyltrisiloxane within 2 hours, stirring for 4 hours at 16 ℃, and removing redundant sulfonyl chloride by reduced pressure suction filtration to obtain 3- (3-chloromethyl) heptamethyltrisiloxane;
(4) slowly adding 3- (3-chloromethyl) heptamethyltrisiloxane into alkynediol polyoxyethylene ether-1500 sodium salt, reacting for 2 hours at 25-40 ℃, and filtering to remove generated sodium chloride to obtain the super-spreading wetting agent W4.
Critical Micelle Concentration (CMC), static surface tension and dynamic surface tension tests were carried out on the super-spreading wetting agents W1-W, the commercial silicone wetting agents W5-W6 and the commercial acetylenic diol wetting agents W7-W8 prepared in the above examples by using a QBZY-1 full-automatic surface tension meter and a Germany KRUSS dynamic surface tension meter, and the results are shown in Table 1.
TABLE 1 CMC values, static surface tension values and dynamic surface tension values of wetting agents W1-W8
Sample name Critical micelle concentration, mmol/L Static surface tension, mN/m Dynamic surface tension, mN/m
W1 0.132 21.3 30.9
W2 0.104 24.2 33.3
W3 0.157 22.3 34.1
W4 0.118 23.8 32.5
W5 0.534 20.5 56.7
W6 0.617 21.1 61.3
W7 0.873 32.0 37.4
W8 0.915 35.2 39.2
As can be seen from Table 1, the CMC value of the superspreading wetting agent is about 1/4 of the CMC value of the commercially available silicone wetting agent and about 1/6 of the CMC value of the commercially available acetylenic diol wetting agent, which facilitates the superspreading of the wetting agent on the substrate. The static surface tension of the super-spreading wetting agents W1-W4 is 21-25 mN/m, is slightly higher than that of commercially available organosilicon wetting agents W5 and W6, but is lower than that of commercially available acetylenic diol wetting agents W7 and W8. Compared with the commercial alkyne diol wetting agents W7 and W8, the difference between the dynamic surface tension and the static surface tension of the superspread wetting agents W1-W4 is slightly enlarged, but the dynamic surface tension value is lower than that of W7 and W8; whereas the dynamic surface tension of the commercially available silicone wetting agents W5 and W6 is extremely high and has not been able to meet wetting of common low surface tension substrates.
The tests for foamability and foam stability of the wetting agents W1-W8 are described as: 50mL of wetting agent aqueous solution with the mass concentration of 1% is taken and placed in a 100mL measuring cylinder for sealing, timing is started after the measuring cylinder is inverted up and down for 10 times, and the volume ratio of the foam to the liquid is read. The specific data are shown in Table 2.
TABLE 2 foaming height of wetting agents W1-W8
Sample name 0 minute, mL 5 min, mL
W1 7 0
W2 9 0
W3 8 1
W4 10 1
W5 18 8.6
W6 21 7.4
W7 4 0
W8 5 0
As can be seen from Table 2, the super-spreading wetting agents prepared by the present invention have much lower foaming properties than the commercially available silicone wetting agents W5 and W6, but slightly higher foaming properties than the commercially available acetylenic diol wetting agents; after standing for 5 minutes, the superspreading wetting agents W1-W2 and the commercial acetylene glycol wetting agents W7 and W8 are basically free of foams, a small amount of air bubbles remain in the superspreading wetting agents W3-W4, and a large amount of air bubbles still remain in the commercial organosilicon wetting agents W5 and W6 although the height of the air bubbles is obviously reduced, so that the results show that the superspreading wetting agents are poor in foam stability, easy to break and close to the commercial acetylene glycol wetting agents, but are superior to the commercial organosilicon wetting agents.
The above description is only an example of the present invention, and not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention in the light of the present specification are included in the scope of the present invention.

Claims (5)

1. A superspreading wetting agent characterized by: the general structural formula of the super-spreading wetting agent is as follows:
wherein R is1And R2Are respectively one of hydrogen, methyl and n-butyl, and R1And R2Not hydrogen at the same time;
R3and R4Are respectively as
Figure 575859DEST_PATH_IMAGE002
C is an integer of 0-15, d is an integer of 0-6, and c + d is more than or equal to 2 and less than or equal to 15;
R5is one of methylene and trimethylene;
the preparation method of the super-spreading wetting agent comprises the following steps:
(1) adding 0.001-0.006 mol of catalyst into 1 mol of alkynyl compound subjected to molecular sieve dehydration under the protection of nitrogen, introducing 4-30 mol of polymerization monomer, heating to 90-120 ℃, keeping the temperature for 3-9 hours, and cooling to 30-40 ℃; introducing the reaction product into a mixed bed type ion exchange column activated by ethanol to remove the catalyst, and obtaining alkynediol polyether;
(2) adding an alcohol solution containing 2 mol of alkali metal alcoholate into alkynediol polyether, heating to 65-80 ℃, keeping a slight boiling state, slowly distilling out alcohol, keeping for 2-6 hours, and then distilling under reduced pressure to remove the alcohol; cooling to 25-35 ℃ to obtain alkali metal salt of the alkynediol polyether;
(3) dripping 2.2-2.8 mol of chlorinating agent into 2 mol of organic silicon compound within 0.5-2 hours, stirring for 2-4 hours at 0-30 ℃, and removing the redundant chlorinating agent by vacuum filtration to obtain the chloride of the organic silicon compound;
(4) adding the chloride of the silicon compound obtained in the step (3) into the alkali metal salt of the alkynediol polyether obtained in the step (2), reacting for 2-5 hours at 25-40 ℃, and filtering to remove generated solid salt to obtain a super-spreading wetting agent;
wherein the alkynyl compound is one of 3-hexyne-2, 5-diol, 2, 5-dimethyl-3-hexyne-2, 5-diol and 5, 8-dimethyl-6-dodecyne-5, 8-diol;
the catalyst is one of zinc hexacyanocobaltate, potassium hydroxide and lithium hydroxide;
the polymerized monomer is one or a combination of two of ethylene oxide and propylene oxide;
the alkali metal alcoholate is one or a combination of sodium methoxide, potassium methoxide, sodium ethoxide and potassium ethoxide;
the organic silicon compound is one of 3- (3-hydroxymethyl) heptamethyltrisiloxane and 3- (3-hydroxypropyl) heptamethyltrisiloxane;
the chlorinating agent is one of thionyl chloride and sulfuryl chloride.
2. The superspreading wetting agent according to claim 1, wherein the superspreading wetting agent is prepared by the following steps:
(1) adding 0.001 mol of catalyst lithium hydroxide into 1 mol of 5, 8-dimethyl-6-dodecyne-5, 8-diol dehydrated by a molecular sieve under the protection of nitrogen, introducing 8 mol of ethylene oxide, heating to 90 ℃, keeping the temperature for 3 hours, and cooling to 40 ℃; introducing the reaction product into an ethanol activated mixed bed type ion exchange column to remove the catalyst, and obtaining acetylene glycol polyoxyethylene ether-0400;
(2) adding a methanol solution containing 2 mol of potassium methoxide into acetylene glycol polyoxyethylene ether-0400, heating to 65 ℃, keeping the temperature slightly boiling, slowly distilling out methanol, keeping for 2 hours, and then distilling under reduced pressure to remove residual methanol; cooling to 25 ℃ to obtain sylvite of alkynediol polyoxyethylene ether-0400;
(3) dropwise adding 2.2 mol of sulfonyl chloride into 2 mol of 3- (3-hydroxypropyl) heptamethyltrisiloxane within 2 hours, stirring for 4 hours at 10 ℃, and removing redundant sulfonyl chloride by vacuum filtration to obtain 3- (3-chloropropyl) heptamethyltrisiloxane;
(4) slowly adding 3- (3-chloropropyl) heptamethyltrisiloxane into acetylene glycol polyoxyethylene ether-0400 potassium salt, reacting for 2 hours at 40 ℃, and filtering to remove generated potassium chloride to obtain the super-spreading wetting agent W1.
3. The superspreading wetting agent according to claim 1, wherein the superspreading wetting agent is prepared by the following steps:
(1) adding 0.004 mol of catalyst potassium hydroxide into 1 mol of 3-hexyne-2, 5-diol dehydrated by a molecular sieve under the protection of nitrogen, introducing 12 mol of propylene oxide, heating to 115 ℃, keeping the temperature for 7 hours, and cooling to 35 ℃; introducing the reaction product into a mixed bed type ion exchange column activated by ethanol to remove the catalyst, and obtaining the alkynediol polyoxypropylene ether-0006;
(2) adding an ethanol solution containing 2 mol of sodium ethoxide into alkynediol polyoxypropylene ether-0006, heating to 80 ℃, keeping the temperature slightly boiling, slowly distilling out ethanol, keeping for 4 hours, and then distilling under reduced pressure to remove residual ethanol; cooling to 25 ℃ to obtain alkynediol polyoxypropylene ether-0006 sodium salt;
(3) dropwise adding 2.8 mol of thionyl chloride into 2 mol of 3- (3-hydroxymethyl) heptamethyltrisiloxane within 0.5 hour, stirring for 2 hours at 30 ℃, and carrying out vacuum filtration to remove excessive thionyl chloride to obtain 3- (3-chloromethyl) heptamethyltrisiloxane;
(4) adding 3- (3-chloromethyl) heptamethyltrisiloxane into alkynediol polyoxypropylene ether-0006 sodium salt, reacting for 5 hours at 25 ℃, and filtering to remove generated sodium chloride to obtain the super-spreading wetting agent W2.
4. The superspreading wetting agent according to claim 1, wherein the superspreading wetting agent is prepared by the following steps:
(1) adding 0.005mol of catalyst zinc hexacyanocobaltate into 1 mol of 2, 5-dimethyl-3-hexyne-2, 5-diol dehydrated by a molecular sieve under the protection of nitrogen, introducing 22 mol of ethylene oxide and 8 mol of propylene oxide, heating to 120 ℃, keeping the temperature for 9 hours, and cooling to 35 ℃; introducing the reaction product into a mixed bed type ion exchange column activated by ethanol to remove the catalyst, and obtaining alkynediol polyoxyethylene polyoxypropylene ether-1104;
(2) adding an ethanol solution containing 1 mol of potassium ethoxide and an ethanol solution containing 1 mol of potassium methoxide into alkynediol polyoxyethylene polyoxypropylene ether-1104, heating to 65 ℃, keeping the mixture in a slightly boiling state for 2 hours, slowly distilling out methanol, heating to 78 ℃ after the methanol is basically distilled out, slowly distilling out the ethanol, keeping for 4 hours, and distilling under reduced pressure to remove residual ethanol; cooling to 30 ℃ to obtain sylvite of alkynediol polyoxyethylene polyoxypropylene ether-1104;
(3) dropwise adding 2.5 mol of thionyl chloride into 2 mol of 3- (3-hydroxypropyl) heptamethyltrisiloxane within 1 hour, stirring for 2.5 hours at 0 ℃, and carrying out vacuum filtration to remove redundant thionyl chloride to obtain 3- (3-chloropropyl) heptamethyltrisiloxane;
(4) adding 3- (3-chloropropyl) heptamethyltrisiloxane into alkynediol polyoxyethylene polyoxypropylene ether-1104 potassium salt, reacting for 4 hours at 30 ℃, and filtering to remove generated potassium chloride to obtain the super-spreading wetting agent W3.
5. The superspreading wetting agent according to claim 1, wherein the superspreading wetting agent is prepared by the following steps:
(1) adding 0.002 mol of catalyst lithium hydroxide into 1 mol of 5, 8-dimethyl-6-dodecyne-5, 8-diol dehydrated by a molecular sieve under the protection of nitrogen, introducing 30 mol of ethylene oxide, heating to 105 ℃, keeping the temperature for 9 hours, and cooling to 30 ℃; introducing the reaction product into a mixed bed type ion exchange column activated by ethanol to remove the catalyst, and obtaining alkynediol polyoxyethylene ether-1500;
(2) adding a methanol solution containing 2 mol of sodium methoxide into alkynediol polyoxyethylene ether-1500, heating to 65 ℃, keeping the temperature slightly boiling, slowly distilling out methanol, keeping for 3 hours, and then distilling under reduced pressure to remove residual methanol; cooling to 35 ℃ to obtain alkynediol polyoxyethylene ether-1500 sodium salt;
(3) dropwise adding 2.3 mol of sulfonyl chloride into 2 mol of 3- (3-hydroxymethyl) heptamethyltrisiloxane within 2 hours, stirring for 4 hours at 16 ℃, and removing redundant sulfonyl chloride by reduced pressure suction filtration to obtain 3- (3-chloromethyl) heptamethyltrisiloxane;
(4) slowly adding 3- (3-chloromethyl) heptamethyltrisiloxane into alkynediol polyoxyethylene ether-1500 sodium salt, reacting for 2 hours at 25-40 ℃, and filtering to remove generated sodium chloride to obtain the super-spreading wetting agent W4.
CN201911158548.8A 2019-11-22 2019-11-22 Super-spreading wetting agent and preparation method thereof Withdrawn CN110818890A (en)

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