CN115260543B - Silane coupling polyether silyl ether and preparation method and application thereof - Google Patents
Silane coupling polyether silyl ether and preparation method and application thereof Download PDFInfo
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- CN115260543B CN115260543B CN202210772464.9A CN202210772464A CN115260543B CN 115260543 B CN115260543 B CN 115260543B CN 202210772464 A CN202210772464 A CN 202210772464A CN 115260543 B CN115260543 B CN 115260543B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2371/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2371/02—Polyalkylene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/02—Polyalkylene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5415—Silicon-containing compounds containing oxygen containing at least one Si—O bond
- C08K5/5419—Silicon-containing compounds containing oxygen containing at least one Si—O bond containing at least one Si—C bond
Abstract
The invention discloses a silicon ether of silane coupling polyether, a preparation method and application thereof. The organosilane in the silane coupling polyether can reduce the surface tension of polyether, so that polyether molecules spread and stretch on the surface of the foam film, the combining speed of bubbles is improved, foam formation is inhibited, and the defect of an organosilicon polymer is avoided. The silyl ether is used as a component of a foam inhibition product, has a good foam control effect on a landfill leachate system, and can be also applied to industries of papermaking wet-end white water, adhesives, printing ink and the like. The preparation method is simple, the materials are subjected to crosslinking reaction, a complex reaction flow and harsh reaction conditions are not required, and the product can be used without treatment.
Description
Technical Field
The invention belongs to the field of fine chemical preparations, and particularly relates to a silane coupling polyether silyl ether and a preparation method and application thereof.
Background
Refuse disposal technology is becoming more and more of a public concern, where refuse landfill and refuse incineration are two conventional ways of disposing of refuse, but refuse landfill and incineration plants do not avoid the generation of leachate which is serious to environmental pollution during refuse disposal. The components of the permeate are complex, more foam is generated in the treatment process of the permeate, and the current method for adding the defoamer is an effective method.
Chinese patent CN201010277461.5 discloses a landfill leachate defoamer mainly comprising nonylphenol polyoxyethylene ether, polyoxypropylene polyoxyethylene glycerol ether, alkylphenol polyoxyethylene ether, low carbon alcohol and microbial flocculant; chinese patent CN202110658304.7 discloses the preparation of a landfill leachate defoamer comprising polyether modified polysiloxane, emulsifier, dispersant, thickener, white carbon black, deionized water; chinese patent CN201710669288.5 discloses that by introducing an organic compound synthesized from monounsaturated fatty acid, fatty diacid, alcohol amine as a foam-suppressing synergist, the glyceryl polyether and the linear or branched fatty alcohol polyether with 10-20 carbon atoms are compounded to obtain a landfill leachate defoamer; chinese patent CN201911207332.6 discloses a defoaming agent for landfill leachate, which comprises triethanolamine polyoxyethylene ether monostearate, cocoanut alcohol polyoxyethylene ether, polyoxyethylene glycerol borate fatty acid ester, poly (octyl glycol) mono-sixteen ether, allyl alcohol polyether and other components; chinese patent CN202011350420.4 discloses an organosilicon landfill leachate defoamer, which comprises polyether modified polydimethylsiloxane, nanoscale fumed silica, modified silicone oil, fatty acid polyoxyethylene ester, an emulsifier, a thickener and a biostatic agent. However, the organic silicon defoamer is easy to block a filter screen film due to the problems of hydrophobicity and particle size of the silicon paste, and affects the permeation of landfill leachate; chinese patent CN201910905397.1 discloses that the garbage percolate defoamer is prepared by using polyoxypropylene polyoxyethylene glycerol ether, alkylphenol ethoxylates, water glass, calcium stearate and organic foam suppressor as raw materials through the processes of stirring, mixing and heat preservation; chinese patent CN202111464578.9 discloses a landfill leachate defoamer using fatty acid polyether ester, polyether polyol and emulsifying dispersant as main defoamer substances.
However, the foam inhibition function of the defoamers still cannot meet the actual requirements, and a chemical preparation with stronger foam inhibition capability needs to be found.
Disclosure of Invention
In order to overcome the defects in the prior art, the first aim of the invention is to provide the silicon ether of the silane coupling polyether, the silicon ether of the silane coupling polyether is formed by the reaction of the polyether and the silane, and the organosilane can reduce the surface tension of the polyether, is favorable for the spreading and stretching of polyether molecules on the surface of a bubble film, so that the bubble merging speed is improved, and the foam inhibition level of the silicon ether molecules is also improved.
The second object of the invention is to provide a preparation method of the silane coupling polyether silyl ether.
The third object of the present invention is to provide the use of the above-mentioned silane-coupled polyether silyl ether.
One of the purposes of the invention can be achieved by adopting the following technical scheme:
the silyl ether of the silane coupling polyether comprises the following raw materials in percentage by mass:
further, the silyl ether of the silane coupling polyether comprises the following raw materials in percentage by mass:
further, the fatty alcohol polyether has a structure shown in a general formula (1):
R 1 O(EO) a (PO) b H;
general formula (1)
Wherein R is 1 Is a straight-chain or branched hydrocarbon group with 6-30 carbon atoms, a is 0 or an integer of 2-50; b is 0 or an integer of 2-100, and a and b are not 0 at the same time.
Further, the straight-chain or branched hydrocarbon group having 6 to 30 carbon atoms is hexyl, octyl, decyl, octadecyl, eicosyl or octacosyl.
The fatty alcohol polyether in the general formula (1) is formed by reacting fatty alcohol with ethylene oxide and/or propylene oxide, wherein the fatty alcohol is a straight-chain or branched-chain higher alcohol fatty alcohol with 6-30 carbon atoms. Wherein EO is an ethylene oxide reactive group, PO is a propylene oxide reactive group, and the ethylene oxide reactive group can be 0 or 2-50; the propylene oxide reactive groups may be 0 or 2 to 100. When the ethylene oxide reactive group is 0, propylene oxide is not 0, indicating that the aliphatic alcohol polyether is obtained by reacting higher aliphatic alcohol with propylene oxide, wherein the number of propylene oxide polymerization monomers is 2-100; also when the propylene oxide reactive group is 0, the aliphatic alcohol polyether is obtained by reacting a higher aliphatic alcohol with ethylene oxide, wherein the number of ethylene oxide polymerization monomers is 2 to 50; when neither ethylene oxide nor propylene oxide reactive groups are 0, the aliphatic polyether is prepared by copolymerizing a higher aliphatic alcohol with ethylene oxide and propylene oxide.
Further, the polyol polyether has a structure shown in a general formula (2):
R 2 [O(EO) c (PO) d H] e ;
general formula (2)
Wherein R is 2 Is a hydrocarbon group with 2-6 carbon atoms, c and d are 0 or integers with 2-50, and c and d are not 0 at the same time; e is an integer from 2 to 6.
Further, the initiator of the polyol polyether is one or a combination of more than two of ethylene glycol, diethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol, glycerol, pentaerythritol and sorbitan.
Similar to fatty alcohols, polyol polyethers are formed by reacting a polyol with ethylene oxide and/or propylene oxide, the polyol having from 2 to 6 carbon atoms and from 2 to 6 hydroxyl groups, wherein preferably the polyol may be a diol, triol, tetraol.
Further, the silane crosslinking agent has a structure shown in a general formula (3):
(R 3 ) f Si(OR 4 )g;
general formula (3)
Wherein R is 3 Alkyl, alkenyl, aryl, alkylaryl having 1 to 18 carbon atoms and alkyl, alkenyl, aryl, alkylaryl having 1 to 18 carbon atoms substituted with amino groups;
R 4 is a straight chain or isomeric alkyl group having 1 to 4 carbon atoms;
f is 0, 1,2 or 3; g is 1,2, 3 or 4, and f+g=4.
Further, the silane crosslinking agent is one or more of methyltrimethoxysilane, ethyltrimethoxysilane, propyltrimethoxysilane, butyltrimethoxysilane, hexyltrimethoxysilane, octyltrimethoxysilane, methyltriethoxysilane, ethyltriethoxysilane, butyltriethoxysilane, hexyltriethoxysilane, octyltriethoxysilane, methyltributoxysilane, ethyltributoxysilane, propyltributoxysilane, butyltributoxysilane, hexyltributoxysilane, octyltributoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, phenyltributoxysilane, tetraethoxysilane, dibutylaminomethyl tributoxysilane, cyclohexylaminomethyltrimethoxysilane, cyclohexylaminomethyltriethoxysilane, aminoethylaminopropyl trimethoxysilane, aminoethylaminopropyl triethoxysilane, 3-dimethylaminopropyl aminomethyltrimethoxysilane, morpholinomethyl trialkoxysilane, dibutylaminomethyltriethoxysilane, morpholinomethyl triisopropoxy silane, and linylmethyl triethoxysilane.
Silane crosslinker, wherein R 4 Is a straight-chain OR isomeric alkyl radical having 1 to 4 carbon atoms, si (OR) 4 ) f OR in the radical 4 Will hydrolyze in the presence of water, si (OR 4 ) f The silanol is generated by the groups, the alcoholic hydroxyl groups in the silanol can be copolymerized and crosslinked with the aliphatic alcohol polyether and the polyol polyether, and the organosilane structure is connected into polyether molecules, so that the surface tension of the polyether can be reduced through the organosilane, the polyether molecules can be spread and stretched on the surface of a bubble film, the bubble merging speed can be improved, and the foam inhibition performance of the polyether is improved.
Further, the catalyst is an acidic catalyst; preferably, the acid catalyst is one or a combination of more than two of sulfuric acid, hydrochloric acid, phosphoric acid, acetic acid and trifluoro boric acid.
Further, the inhibitor is one or a combination of more than two of methanol, ethanol, isopropanol and isobutanol.
Further, the water is deionized water, and preferably, the sum of the contents of calcium ions and magnesium ions in the deionized water is not more than 20ppm.
The silane crosslinking agent needs to be hydrolyzed under aqueous conditions, and thus a certain amount of water needs to be present in the reaction system. And silanol formed after the silane is hydrolyzed is easy to combine with calcium and magnesium ions, so that the content of the calcium and magnesium ions in water is further limited to be less than 20ppm, and the hydrolyzed silane cross-linking agent can fully realize copolymerization and cross-linking with polyether to form a silicon ether compound.
The second aim of the invention can be achieved by adopting the following technical scheme:
a process for preparing the silyl ether of silane-coupled polyether as claimed in any one of the preceding claims, which comprises mixing fat
Uniformly stirring alcohol polyether, polyol polyether, inhibitor, water and catalyst, adding a silane cross-linking agent, and reacting for 2-8 hours; and regulating the pH value of the system to 8.0-10.0, and continuing the reaction to obtain the silyl ether of the silane coupling polyether.
Further, the reaction system is warmed to 50-80 ℃ before adding the silane crosslinking agent.
Further, the silane crosslinking agent is added dropwise within 30-180 min.
Further, after the pH value of the system is regulated, the reaction system is heated to 110-150 ℃ and then reacts for 2-10 hours to obtain the silyl ether of the silane coupling polyether.
The third object of the invention can be achieved by adopting the following technical scheme:
use of a silyl ether of a silane-coupled polyether as defined in any of the preceding claims in a foam-inhibiting product.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention discloses a silicon ether of silane coupling polyether, which is prepared by mixing fatty alcohol and polyol polyether according to a certain proportion, and then copolymerizing and crosslinking with a silane crosslinking agent in the presence of water; the organosilane reduces the surface tension of polyether, is favorable for spreading and stretching polyether molecules on the surface of a film of the foam, further improves the speed of bubble combination, improves the level of the silicon ether for inhibiting the foam, and does not bring about the defect of organosilicon polymers. The obtained silyl ether is used as a component of a foam inhibition product, has a good foam control effect on a landfill leachate system, and can be also applied to industries such as papermaking wet-end white water, adhesives, printing ink and the like.
2. According to the preparation method of the silane coupling polyether silyl ether, the materials are subjected to crosslinking reaction, a complex reaction flow and harsh reaction conditions are not required, and the product can be used without treatment.
Detailed Description
The present invention will be further described with reference to the following specific embodiments, and it should be noted that, on the premise of no conflict, new embodiments may be formed by any combination of the embodiments or technical features described below.
In actual handling, the defoamers are of a wide variety, including silicones, polyethers, polyether esters, mineral oils, fatty alcohols, even tributyl phosphate and the like. However, considering the treatment process specificity of landfill leachate, polyether or modified polyether or a compound defoamer formed by compounding other substances with polyether as a main component is relatively approved in the industry at present. The defoaming performance of polyether is improved through compounding, esterification and organosilicon modification, but the requirements of industrial production are still not met.
The inventor of the application finds through a large number of experiments that after fatty alcohol and polyol polyether are mixed according to a certain proportion, copolymerization crosslinking is carried out with a silane crosslinking agent in the presence of water, the defoaming effect of the obtained silicon ether can be obviously improved, and the defect of an organosilicon polymer is avoided. The foam control agent has a good foam control effect in a landfill leachate system, and can be applied to industries of papermaking wet-end white water, adhesives, printing ink and the like. Therefore, the invention provides a silane coupling polyether silyl ether, and a preparation method and application thereof
Example 1
Into a reaction flask was charged 30 parts of hexanol polyether C 6 H 13 O(PO) 6 0H, 40 parts of glycerol polyether C 3 H 5 [O(EO) 25 (PO) 25 H] 3 11.5 parts of methanol, 15 parts of deionized water and 0.5 part of hydrochloric acid, stirring is started, the temperature is increased to 60 ℃,3 parts of butyl trimethoxy silane is dropwise added into a reaction bottle within 50min, and the reaction is carried out for 4h under the temperature condition after the dropwise addition; and then regulating the pH value of the system to 8.0, raising the temperature to 120 ℃, reacting for 3 hours, and filtering to obtain a sticky substance which is the silyl ether of the silane coupling polyether.
Example 2
Into a reaction flask was charged 50 parts of stearyl polyether C 18 H 37 O(EO) 48 H. 25 parts of diethylene glycol polyether C 4 H 8 [O(EO) 12 (PO) 18 H] 2 7 parts of isobutanol, 10 parts of deionized water and 3 parts of acetic acid, stirring, raising the temperature to 80 ℃, dropwise adding 5 parts of ethyltriethoxysilane into a reaction bottle within 120min, and reacting for 6h under the temperature condition after the dropwise adding is finished; and then regulating the pH value of the system to 9.0, raising the temperature to 130 ℃, reacting for 4 hours, and filtering to obtain a sticky substance which is the silyl ether of the silane coupling polyether.
Example 3
70 parts of octanol polyether C is added into a reaction bottle 8 H 17 O(EO) 10 (PO) 3 0H, 10 parts of pentaerythritol polyether C 5 H 8 [O(EO) 12 (PO) 18 H] 4 11 parts of ethanol, 5 parts of deionized water and 2 parts of trifluoro boric acid, stirring is started, the temperature is increased to 70 ℃,2 parts of octyl triethoxysilane is added dropwise into a reaction bottle within 50min, and the reaction is carried out for 3h under the temperature condition after the dropwise addition is finished; and then regulating the pH value of the system to 9, raising the temperature to 110 ℃, reacting for 6 hours, and filtering to obtain a sticky substance which is the silicon ether of the silane coupling polyether.
Example 4
Into a reaction flask was charged 55 parts of arachidyl alcohol polyether C 20 H 41 O(EO) 30 (PO) 8 0H, 30 parts of butanediol polyether C 4 H 8 [O(EO) 20 (PO) 5 H] 2 4 parts of isopropanol, 7 parts of deionized water and 0.1 part of phosphoric acid, stirring is started, the temperature is increased to 80 ℃, 3.9 parts of methyltriethoxysilane is dropwise added into a reaction bottle within 120min, and the reaction is carried out for 5h under the temperature condition after the dropwise addition is finished; and then regulating the pH value of the system to 10.0, raising the temperature to 140 ℃, reacting for 6 hours, and filtering to obtain a sticky substance which is the silyl ether of the silane coupling polyether.
Example 5
40 parts of decyl polyether C were added to the reaction flask 10 H 21 O(EO) 15 (PO) 20 H. 45 parts of sorbitan polyether C 6 H 8O [O(PO) 48 H] 6 2 parts of methanol, 8 parts of deionized water and 4 parts of sulfuric acid, stirring is started, the temperature is increased to 65 ℃, 1 part of octyl tributoxy silane is added dropwise into a reaction bottle within 130min, and the temperature is maintained after the dropwise additionReacting for 6h; and then regulating the pH value of the system to 9.0, raising the temperature to 120 ℃, reacting for 9 hours, and filtering to obtain a sticky substance which is the silyl ether of the silane coupling polyether.
Example 6
Into a reaction flask was added 20 parts of octanol polyether C 8 H 17 O(EO) 50 (PO) 3 H. 50 parts ofEthylene glycol polyetherC 2 H 4 [O(EO) 3 (PO) 20 H] 2 15 parts of ethanol, 6 parts of deionized water and 5 parts of hydrochloric acid, stirring is started, the temperature is increased to 60 ℃, 4 parts of octyl tributoxy silane is dropwise added into a reaction bottle within 135min, and the reaction is carried out for 8h under the temperature condition after the dropwise addition is finished; and then regulating the pH value of the system to 8.5, raising the temperature to 110 ℃, reacting for 10 hours, and filtering to obtain a sticky substance which is the silyl ether of the silane coupling polyether.
Example 7
Into a reaction flask was charged 27 parts of octacosanol polyether C 28 H 57 O(EO) 45 (PO) 15 H. 45 parts of ethylene glycol polyether C 2 H 4 [O(EO) 40 H] 2 Stirring 10 parts of ethanol, 9 parts of deionized water and 5 parts of phosphoric acid, raising the temperature to 70 ℃, dropwise adding 4 parts of octyl triethoxysilane into a reaction bottle within 120min, and reacting for 7h under the temperature condition after the dropwise adding is finished; and then regulating the pH value of the system to 9.5, raising the temperature to 120 ℃, reacting for 10 hours, and filtering to obtain a sticky substance which is the silyl ether of the silane coupling polyether.
Comparative example 1
Into a reaction flask was charged 41 parts of decyl alcohol polyether C 10 H 21 O(EO) 15 (PO) 20 H. 45 parts of sorbitan polyether C 6 H 8O [O(PO) 48 H] 6 2 parts of methanol, 8 parts of deionized water and 4 parts of sulfuric acid, stirring is started, the temperature is increased to 65 ℃, and the reaction is carried out for 6 hours under the temperature condition; then the pH value of the system is regulated to 9.0, the temperature is increased to 120 ℃, the reaction is carried out for 9 hours, and the obtained sticky matter is filtered.
Comparative example 2
Into a reaction flask was added 80 parts of octanol polyether C 8 H 17 O(EO) 10 (PO) 30 H. 11 parts ofEthanol, 5 parts of deionized water and 2 parts of trifluoro boric acid, stirring, raising the temperature to 70 ℃, dropwise adding 2 parts of octyl triethoxysilane into a reaction bottle within 50min, and reacting for 3h under the temperature condition after the dropwise adding is finished; then the pH value of the system is regulated to 9.0, the temperature is increased to 110 ℃, the reaction is carried out for 6 hours, and the obtained sticky matter is filtered.
Comparative example 3
Into a reaction flask was added 80 parts pentaerythritol polyether C 5 H 8 [O(EO) 20 H] 4 11 parts of methanol, 5 parts of deionized water and 2 parts of trifluoro boric acid, stirring is started, the temperature is increased to 70 ℃,2 parts of isobutyl triethoxysilane is added dropwise into a reaction bottle within 120min, and the reaction is carried out for 5h under the temperature condition after the dropwise addition is finished; then the pH value of the system is regulated to 9.0, the temperature is increased to 110 ℃, the reaction is carried out for 5 hours, and the obtained sticky matter is filtered.
Comparative example 4
70 parts of octanol polyether C is added into a reaction bottle 8 H 17 O(EO) 10 (PO) 30 H. 10 parts of pentaerythritol polyether C 5 H 8 [O(EO) 20 H] 4 11 parts of ethanol, 5 parts of deionized water and 2 parts of trifluoro boric acid, stirring is started, the temperature is increased to 70 ℃,2 parts of octyl triethoxysilane is added dropwise into a reaction bottle within 50min, and the reaction is carried out for 3h under the temperature condition after the dropwise addition is finished; then the pH value of the system is regulated to 9.0, the temperature is increased to 110 ℃, the reaction is carried out for 6 hours, and the obtained sticky matter is filtered.
Comparative example 5
Octanol polyether C 8 H 17 O(EO) 10 (PO) 30 H。
Comparative example 6
Pentaerythritol polyether C 5 H 8 [O(EO) 20 H] 4 。
Test examples
The testing method comprises the following steps: and (3) taking the site landfill leachate as a test medium, and testing the foam inhibition performance of the sample in a bubbling mode. The longer the foam takes to reach the same volume, the better the foam suppression performance of the sample.
Test conditions: (1) temperature: 50 ℃; (2) amount of landfill leachate: 300ml; (3) sample addition amounts of comparative examples 1 to 5 of examples 1 to 7: 30. Mu.L; (4) test flow rate: 5L/min.
The test results are shown in table 1:
table 1 inhibition data for landfill leachate foam by example and comparative polyethers
As can be seen from the test data in Table 1, the silyl ethers of the silane-coupled polyethers of examples 1-7 have a better inhibition of the foaming of the landfill leachate. Using the silyl ethers of the silane-coupled polyethers of examples 1-7, the foam reached a volume of 800ml, which took more than 10 minutes and 23 seconds, and examples 4-5 also reached more than 11 minutes. As comparative examples 5 to 6, the conventional fatty alcohol polyether octanol polyether C was used 8 H 17 O(EO) 10 (PO) 3 0H and polyol polyether pentaerythritol polyether C 5 H 8 [O(EO) 20 H] 4 As suds suppressors, the foam reached the same volume of 800ml, taking less than 4 minutes. It can be seen from comparative examples 1 and 4 that the aliphatic alcohol polyethers and polyol polyethers do not significantly extend the time when the foam reaches the same volume of 800ml without the use of a silane crosslinking agent, indicating that the foam suppressing effect is not improved. Meanwhile, as shown in comparative examples 2 to 3, the aliphatic alcohol polyether octanol polyether C alone 8 H 17 O(EO) 10 (PO) 3 0H and polyol polyether pentaerythritol polyether C 5 H 8 [O(EO) 20 H] 4 The product obtained by respectively reacting with the silane cross-linking agent, the catalyst, water and the inhibitor is used as a foam inhibitor, when the foam reaches 800ml with the same volume, the consumed time is 4 '28' and 5 '15', and compared with the single use of comparative examples 5-6, the time is prolonged to a certain extent, which indicates that the organosilane can improve the foam inhibition effect of the aliphatic alcohol polyether or the polyol polyether. Meanwhile, by comparing comparative examples 1 to 6 with examples 1 to 7, it is evident that the silane coupling agent works together with the aliphatic polyether and the polyol polyether to effect copolymerizationCrosslinking, reducing the surface tension of polyether, enabling polyether molecules to spread and stretch on the surface of a foam membrane, improving the speed of bubble combination and improving the foam inhibition capability of the polyether defoamer.
In summary, the silyl ether of the silane coupling polyether is prepared by mixing fatty alcohol and polyol polyether according to a certain proportion, and then copolymerizing and crosslinking the mixture with a silane crosslinking agent in the presence of water; the organosilane reduces the surface tension of polyether, is favorable for spreading and stretching polyether molecules on the surface of a film of the foam, further improves the speed of bubble combination, improves the level of the silicon ether for inhibiting the foam, and does not bring about the defect of organosilicon polymers. The obtained silyl ether is used as a component of a foam inhibition product, has a good foam control effect on a landfill leachate system, and can be also applied to industries such as papermaking wet-end white water, adhesives, printing ink and the like. The preparation method is simple, the materials are subjected to crosslinking reaction, a complex reaction flow and harsh reaction conditions are not required, and the product can be used without treatment
The above embodiments are only preferred embodiments of the present invention, and the scope of the present invention is not limited thereto, but any insubstantial changes and substitutions made by those skilled in the art on the basis of the present invention are intended to be within the scope of the present invention as claimed.
Claims (7)
1. The silane coupling polyether silyl ether is characterized by comprising the following raw materials in percentage by mass:
the fatty alcohol polyether has a structure shown in a general formula (1):
R 1 O(EO) a (PO) b H;
general formula (1)
Wherein R is 1 Is a straight-chain or branched hydrocarbon group with 6-30 carbon atoms, a is 0 or an integer of 2-50; b is 0 or an integer of 2-100, a, bNot simultaneously 0;
the polyol polyether has a structure shown in a general formula (2):
R 2 [O(EO) c (PO) d H] e ;
general formula (2)
Wherein R is 2 Is a hydrocarbon group with 2-6 carbon atoms, c and d are 0 or integers with 2-50, and c and d are not 0 at the same time; e is an integer from 2 to 6; the initiator of the polyol polyether is one or a composition of more than two of ethylene glycol, diethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol, glycerol, pentaerythritol and sorbitan;
the inhibitor is one or more of methanol, ethanol, isopropanol and isobutanol.
2. The silane-coupled polyether silyl ether of claim 1, wherein the silane cross-linking agent has a structure represented by general formula (3):
(R 3 ) f Si(OR 4 ) g ;
general formula (3)
Wherein R is 3 Alkyl, alkenyl, aryl, alkylaryl having 1 to 18 carbon atoms and alkyl, alkenyl, aryl, alkylaryl having 1 to 18 carbon atoms substituted with amino groups;
R 4 is a straight chain or isomeric alkyl group having 1 to 4 carbon atoms;
f is 0, 1,2 or 3; g is 1,2, 3 or 4, and f+g=4.
3. The silyl ether of a silane coupling polyether of claim 2, wherein the silane cross-linking agent is one or more of methyltrimethoxysilane, ethyltrimethoxysilane, propyltrimethoxysilane, butyltrimethoxysilane, hexyltrimethoxysilane, octyltrimethoxysilane, methyltriethoxysilane, ethyltriethoxysilane, butyltriethoxysilane, hexyltriethoxysilane, octyltriethoxysilane, methylttributoxysilane, ethyltributoxysilane, propyltributoxysilane, butyltributoxysilane, hexyltributoxysilane, octyltributoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, vinyltributoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, phenyltributoxysilane, tetraethoxysilane, dibutylaminomethyltributoxysilane, cyclohexylaminomethyltriethoxysilane, aminoethylaminopropyl trimethoxysilane, aminoethylaminopropyl triethoxysilane, 3-dimethylaminopropylaminomethyl trimethoxysilane, morpholinomethyltrialkoxysilane, dibutylaminomethyltriethoxysilane, morpholinomethyl triisopropoxysilane, and trilinol methylsilane.
4. The silane-coupled polyether silyl ether of claim 1, wherein the catalyst is one or a combination of more than two of sulfuric acid, hydrochloric acid, phosphoric acid, acetic acid and trifluoro boric acid.
5. A process for preparing the silyl ether of a silane-coupled polyether as claimed in any one of claims 1 to 4,
uniformly stirring fatty alcohol polyether, polyol polyether, inhibitor, water and catalyst, adding a silane cross-linking agent, and reacting for 2-8 hours; and regulating the pH value of the system to 8.0-10.0, and continuing the reaction to obtain the silyl ether of the silane coupling polyether.
6. The method for preparing a silane-coupled polyether silyl ether according to claim 5, wherein,
before adding the silane crosslinking agent, heating the reaction system to 50-80 ℃;
the silane crosslinking agent is added dropwise within 30-180 min;
after the pH value of the system is regulated, the reaction system is heated to 110-150 ℃ and then reacts for 2-10 hours to obtain the silicon ether of the silane coupling polyether.
7. Use of the silyl ether of a silane-coupled polyether as defined in any of claims 1 to 4 in foam-inhibiting products.
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