CN111484630A - 一种聚合物乳液型消泡剂及其制备方法 - Google Patents
一种聚合物乳液型消泡剂及其制备方法 Download PDFInfo
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- CN111484630A CN111484630A CN202010207349.8A CN202010207349A CN111484630A CN 111484630 A CN111484630 A CN 111484630A CN 202010207349 A CN202010207349 A CN 202010207349A CN 111484630 A CN111484630 A CN 111484630A
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- Prior art keywords
- acrylate
- defoaming agent
- polymer emulsion
- preparation
- polymer
- Prior art date
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- 239000013530 defoamer Substances 0.000 title claims abstract description 45
- 229920000642 polymer Polymers 0.000 title claims abstract description 40
- 239000000839 emulsion Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000013543 active substance Substances 0.000 claims abstract description 25
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 23
- 229920000570 polyether Polymers 0.000 claims abstract description 23
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims abstract description 20
- 239000003054 catalyst Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 13
- 229920000058 polyacrylate Polymers 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 12
- 239000000945 filler Substances 0.000 claims abstract description 10
- 239000002562 thickening agent Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 29
- 239000002518 antifoaming agent Substances 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 230000035484 reaction time Effects 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- 230000002209 hydrophobic effect Effects 0.000 claims description 7
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims description 6
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 6
- 229920002401 polyacrylamide Polymers 0.000 claims description 6
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 5
- CEGOLXSVJUTHNZ-UHFFFAOYSA-K aluminium tristearate Chemical compound [Al+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CEGOLXSVJUTHNZ-UHFFFAOYSA-K 0.000 claims description 5
- 229940063655 aluminum stearate Drugs 0.000 claims description 5
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 5
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 4
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 4
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 4
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 4
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 4
- PBOSTUDLECTMNL-UHFFFAOYSA-N lauryl acrylate Chemical compound CCCCCCCCCCCCOC(=O)C=C PBOSTUDLECTMNL-UHFFFAOYSA-N 0.000 claims description 4
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 4
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- WYGWHHGCAGTUCH-UHFFFAOYSA-N 2-[(2-cyano-4-methylpentan-2-yl)diazenyl]-2,4-dimethylpentanenitrile Chemical compound CC(C)CC(C)(C#N)N=NC(C)(C#N)CC(C)C WYGWHHGCAGTUCH-UHFFFAOYSA-N 0.000 claims description 2
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- 239000006229 carbon black Substances 0.000 claims description 2
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 2
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 2
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- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims 1
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- GVNVAWHJIKLAGL-UHFFFAOYSA-N 2-(cyclohexen-1-yl)cyclohexan-1-one Chemical compound O=C1CCCCC1C1=CCCCC1 GVNVAWHJIKLAGL-UHFFFAOYSA-N 0.000 description 16
- 101150065749 Churc1 gene Proteins 0.000 description 16
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- VTYAMJBBERNKSU-UHFFFAOYSA-N ethane-1,2-diamine;octadecanamide Chemical compound NCCN.CCCCCCCCCCCCCCCCCC(N)=O.CCCCCCCCCCCCCCCCCC(N)=O VTYAMJBBERNKSU-UHFFFAOYSA-N 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
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- HGUFODBRKLSHSI-UHFFFAOYSA-N 2,3,7,8-tetrachloro-dibenzo-p-dioxin Chemical compound O1C2=CC(Cl)=C(Cl)C=C2OC2=C1C=C(Cl)C(Cl)=C2 HGUFODBRKLSHSI-UHFFFAOYSA-N 0.000 description 2
- ZFHJDLKOLPSSQL-UHFFFAOYSA-N 3-(tert-butylperoxymethyl)heptane Chemical compound CCCCC(CC)COOC(C)(C)C ZFHJDLKOLPSSQL-UHFFFAOYSA-N 0.000 description 2
- ZVFDTKUVRCTHQE-UHFFFAOYSA-N Diisodecyl phthalate Chemical compound CC(C)CCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC(C)C ZVFDTKUVRCTHQE-UHFFFAOYSA-N 0.000 description 2
- 150000001408 amides Chemical class 0.000 description 2
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- 239000012847 fine chemical Substances 0.000 description 2
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- 239000007788 liquid Substances 0.000 description 2
- 239000002480 mineral oil Substances 0.000 description 2
- 235000010446 mineral oil Nutrition 0.000 description 2
- FSAJWMJJORKPKS-UHFFFAOYSA-N octadecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C=C FSAJWMJJORKPKS-UHFFFAOYSA-N 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- GAWIXWVDTYZWAW-UHFFFAOYSA-N C[CH]O Chemical group C[CH]O GAWIXWVDTYZWAW-UHFFFAOYSA-N 0.000 description 1
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- 150000001336 alkenes Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
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- 230000002035 prolonged effect Effects 0.000 description 1
- AZIQALWHRUQPHV-UHFFFAOYSA-N prop-2-eneperoxoic acid Chemical compound OOC(=O)C=C AZIQALWHRUQPHV-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- B01D—SEPARATION
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- 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
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/22—Oxides; Hydroxides of metals
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K5/098—Metal salts of carboxylic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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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
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
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- D21H21/12—Defoamers
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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
- C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2351/08—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- 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
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/24—Homopolymers or copolymers of amides or imides
- C08J2433/26—Homopolymers or copolymers of acrylamide or methacrylamide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K2003/222—Magnesia, i.e. magnesium oxide
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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
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- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K2003/2241—Titanium dioxide
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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
- C08K2201/00—Specific properties of additives
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- C08K2201/006—Additives being defined by their surface area
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Toxicology (AREA)
- Degasification And Air Bubble Elimination (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Macromonomer-Based Addition Polymer (AREA)
Abstract
本发明提供了一种聚合物乳液型消泡剂及其制备方法，组分包括活性物、填料粒子、水、增稠剂，其中活性物由丙烯酸酯，烯丙基聚醚，催化剂组成，通过在丙烯酸酯聚合物链段中引入含有亲水官能团的烯丙基聚醚，合成过程中烯丙基聚醚的引入解决了传统丙烯酸酯合成过程中使用甲苯等有害溶剂带来的环保问题；双键加成反应形成一种自乳化功能的聚合物高分子，可在水中进行乳化，形成不同粒径范围的乳液；聚合物乳液由于自身可实现自乳化形成乳液，解决了传统有机硅乳液型消泡剂使用一些乳化剂所带来的漂油，析出，破乳等一系列问题。
Description
技术领域
本发明涉及一种聚合物乳液型消泡剂及制备方法，聚合物乳液是重要精细化学品添加剂，因此，本发明隶属于精细化工制剂技术领域。
背景技术
造纸是国民经济生产中的重点工业。在造纸工业中，常常用到多种表面活性剂，例如消泡剂。绝大多数工业生产中泡沫会带来极大的危害，例如降低机器的工作效率、延误劳动时间、影响最终产品的质量等。消除有害泡沫的方法一般采用添加消泡剂的方式。消泡组合物的不同，消泡剂分为非硅型和有机硅类等几种主要类型。与其他消泡剂相比，有机硅类消泡剂化学性能稳定，耐化学品稳定，副作用小，同时在用量很低的情况下也有很好的瞬间消泡能力，因而，很受青睐。而非硅消泡剂是以矿物油、聚醚、酰胺或脂肪醇、丙烯酸酯为活性物，在大量的使用时，活性物酰胺会逐渐聚集，凝结，在纸张上残留斑点；且矿物油在长时间的高温情况下会产生四氯二苯并-p-二恶英(TCDD)有害物质，危害人身安全及环境安全。有机硅消泡剂是以聚硅氧烷、填料等为活性物，长时间的使用会导致疏水粒子的团聚，后附着在纸张上，形成硅斑，造成纸张质量下降。
专利US5152925A介绍的是以一种聚丙烯酸酯作为主要消泡活性物质的消泡剂，其中丙烯酸酯聚合物主要以含有羟基的丙烯酸酯类单体在溶剂邻苯二甲酸二异癸酯(DIDP)或DIOP等溶剂中制备的丙烯酸酯聚合物作为主要活性物质，应用于造纸黑液洗涤和其他造纸工序。专利CN102428142B中同样提到以丙烯酸酯聚合物作为活性物质制备本体型消泡剂，其中丙烯酸酯聚合物由丙烯酸异辛酯、丙烯酸羟基酯以及丙烯酸等单体在聚丁烯或聚醚溶剂等中制备，将制备的丙烯酸酯聚合物作为消泡剂的主要活性成分，并和白炭黑、烷基硅油等消泡助剂复配，应用于石油开采、水处理、涂料工业和油墨、食品和饮料加工、钻井业、纺织业、造纸等行业。此类消泡剂的出现可以解决传统有机硅消泡剂硅析出残留问题，但是目前技术制备的消泡剂消抑泡性能仍有很大的提升空间。因此，提高丙烯酸酯聚合物消泡剂的消抑泡性能将有重要意义。
发明内容
本发明解决上述存在的问题，提出一种基于聚合物为活性物的乳液型消泡剂。本发明的优势：
（1）通过在丙烯酸酯聚合物链段中引入含有亲水官能团的烯丙基聚醚，通过双键加成反应形成一种自乳化功能的聚合物高分子，通过催化剂的含量和反应时间调整分子量的大小，使其具有一定范围的粘度，可在水中进行乳化，形成不同粒径范围的乳液。
（2）高分子聚合物中所引入的烯丙基聚醚，利用其结构中(OCH2CH2)a和(OCH2CHCH3)b对分子结构进行调整亲水疏水平衡值（HLB），(OCH2CH2)a增加可显著改善亲水性能，(OCH2CHCH3)b可调节疏水性能，从而实现分子结构的自乳化形成乳液。
（3）在合成过程中，烯丙基聚醚粘度较小，既作为反应单体，又实现了反应溶剂的作用，解决了传统丙烯酸酯合成过程中使用甲苯等有害溶剂带来的环保问题。
（4）聚合物乳液由于自身可实现自乳化形成乳液，解决了传统有机硅乳液型消泡剂使用一些乳化剂所带来的漂油，析出，破乳等一系列问题。
为实现上述效果，本发明的一种聚合物乳液型消泡剂及制备方法技术方案如下：
一种聚合物乳液型消泡剂由以下组分组成：活性物占消泡剂总质量的10-35%，填料粒子占消泡剂总质量的3-8%，水占消泡剂总质量的60-85%，增稠剂占消泡剂总质量的0.5-3%；
一种聚合物乳液型消泡剂及其制备方法，所述活性物由丙烯酸酯，烯丙基聚醚，催化剂组成，其中丙烯酸酯占活性物总质量的29-70%，烯丙基聚醚占活性物总质量的29-70%，催化剂占活性物总质量的0.5-2%；
一种聚合物乳液型消泡剂及制备方法，所述丙烯酸酯选自丙烯酸羟乙酯、丙烯酸甲酯、丙烯酸乙酯、丙烯酸丁酯、丙烯酸月桂酯、丙烯酸十八酯、丙烯酸异辛酯中的一种或两种以上任意比例混合；
一种聚合物乳液型消泡剂及制备方法，所述填料粒子选自疏水白炭黑、二氧化钛、氧化镁、氧化铝、乙二胺双硬脂酸酰胺(EBS)、硬脂酸铝中的一种或几种；
一种聚合物乳液型消泡剂及制备方法中所述填料粒子比表面积为150～500m2/g；
一种聚合物乳液型消泡剂及其制备方法中所述增稠剂为聚丙烯酰胺、卡波姆、汉生胶、聚丙烯酸酯、甲基纤维素、羧甲基纤维素、羟乙基纤维素、乙基纤维素中一种或几种；
一种聚合物乳液型消泡剂及制备方法，所述烯丙基聚醚的结构通式如下：
CH2=CHCH2(OCH2CH2)a(OCH2CHCH3)b其中a为1-10整数，b为10-100整数。
一种聚合物乳液型消泡剂及制备方法，所述催化剂选自2,2’-偶氮双(2-甲基丙腈)，过氧化2-乙基己基酸叔丁酯，过氧化叔丁基，2,2’-偶氮双(2,4-二甲基戊腈)，2,2’-偶氮双(2-甲基丁腈)、过氧化苯甲酰中一种；
一种聚合物乳液型消泡剂制备方法，包括以下步骤：
（1）活性物的制备：将丙烯酸酯，催化剂加入烧瓶中，搅拌时间30-90min，将上述混合物滴入含有烯丙基聚醚的反应器中，反应温度60-100℃，滴加反应时间为2-8h；
（2）将活性物，填料粒子，增稠剂置于高速搅拌器中，搅拌速度为1500-2500rpm，缓慢滴入水，搅拌时间30-120min后，得到聚合物乳液消泡剂。
具体实施方式
实施例一、
（1）活性物的制备：将10g丙烯酸羟乙酯、19g丙烯酸异辛酯、1g催化剂2,2’-偶氮双(2-甲基丙腈)加入烧瓶中，搅拌时间30min，将上述混合物滴入含有70g烯丙基聚醚CH2=CHCH2(OCH2CH2)(OCH2CHCH3)100的反应器中，反应温度60℃，滴加反应时间为8h；
（2）将10g活性物、8g疏水白炭黑（比表面积为150m2/g）、1g聚丙烯酰胺、2g聚丙烯酸酯置于高速搅拌器中，搅拌速度为1500rpm，缓慢滴入79g的水，搅拌时间120min后，得到聚合物乳液消泡剂，记为A。
实施例二、
（1）活性物的制备：将70g丙烯酸乙酯，1g催化剂过氧化2-乙基己基酸叔丁酯加入烧瓶中，搅拌时间90min，将上述混合物滴入含有29g烯丙基聚醚CH2=CHCH2(OCH2CH2)10(OCH2CHCH3)10的反应器中，反应温度100℃，滴加反应时间为2h；
（2）将35g活性物，3g二氧化钛（比表面积300m2/g），0.5g聚丙烯酰胺置于高速搅拌器中，搅拌速度为2500rpm，缓慢滴入61.5g的水，搅拌时间30min后，得到聚合物乳液消泡剂，记为B。
实施例三、
（1）活性物的制备：将10g丙烯酸月桂酯、35g丙烯酸丁酯，0.5g催化剂过氧化苯甲酰加入烧瓶中，搅拌时间60min，将上述混合物滴入含有54.5g烯丙基聚醚CH2=CHCH2(OCH2CH2)5(OCH2CHCH3)50的反应器中，反应温度80℃，滴加反应时间为5h；
（2）将34g活性物，2g乙二胺双硬脂酸酰胺(比表面积为200 m2/g)，3g硬脂酸铝(比表面积为300 m2/g)，1g汉生胶置于高速搅拌器中，搅拌速度为2000rpm，缓慢滴入60g的水，搅拌时间80min后，得到聚合物乳液消泡剂，记为C。
实施例四、
（1）活性物的制备：将60g丙烯酸甲酯，5g丙烯酸十八酯，2g催化剂2,2’-偶氮双(2-甲基丁腈)加入烧瓶中，搅拌时间50min，将上述混合物滴入含有33g烯丙基聚醚CH2=CHCH2(OCH2CH2)8(OCH2CHCH3)65的反应器中，反应温度70℃，滴加反应时间为4h；
（2）将10.5g活性物，1.5g卡波姆，1.5g氧化镁(比表面积为250 m2/g)，1.5g氧化铝(比表面积为300 m2/g)置于高速搅拌器中，搅拌速度为2300rpm，缓慢滴入85g的水，搅拌时间100min后，得到聚合物乳液消泡剂，记为D。
实施例五、
（1）活性物的制备：将10g丙烯酸羟乙酯，10g丙烯酸异辛酯，10g丙烯酸丁酯，1.5g过氧化叔丁基加入烧瓶中，搅拌时间40min，将上述混合物滴入含有48.5g烯丙基聚醚CH2=CHCH2(OCH2CH2)3(OCH2CHCH3)32的反应器中，反应温度70℃，滴加反应时间为7h；
（2）将22g活性物，6g硬脂酸铝（比表面积为350 m2/g），2g羧甲基纤维素置于高速搅拌器中，搅拌速度为1600rpm，缓慢滴入70g的水，搅拌时间50min后，得到聚合物乳液消泡剂，记为E。
对比例1
（1）活性物的制备：将40g丙烯酸羟乙酯、58g丙烯酸异辛酯、2g催化剂2,2’-偶氮双(2-甲基丙腈)加入烧瓶中，搅拌均匀，升温至反应温度60℃，反应时间为8h；
（2）将10g活性物、8g疏水白炭黑（比表面积为150m2/g）、1g聚丙烯酰胺、2g聚丙烯酸酯置于高速搅拌器中，搅拌速度为1500rpm，缓慢滴入79g的水，搅拌时间120min后，得到聚合物消泡剂，记为F。
对比例2
（1）活性物的制备：将70g丙烯酸乙酯，1g催化剂过氧化2-乙基己基酸叔丁酯加入烧瓶中，搅拌时间90min，将上述混合物滴入含有29g烯丙基聚醚CH2=CHCH2(OCH2CH2)100(OCH2CHCH3)200的反应器中，反应温度100℃，滴加反应时间为2h；
（2）将35g活性物，3g二氧化钛（比表面积300m2/g），0.5g聚丙烯酰胺置于高速搅拌器中，搅拌速度为2500rpm，缓慢滴入61.5g的水，搅拌时间30min后，得到聚合物消泡剂，记为G。
对比例3
（1）活性物的制备：将10g丙烯酸月桂酯、35g丙烯酸丁酯，0.5g催化剂过氧化苯甲酰加入烧瓶中，搅拌时间60min，将上述混合物滴入含有54.5g烯丙基聚醚CH2=CHCH2(OCH2CH2)5(OCH2CHCH3)3的反应器中，反应温度80℃，滴加反应时间为5h；
（2）将34g活性物，2g乙二胺双硬脂酸酰胺(比表面积为200 m2/g)，3g硬脂酸铝(比表面积为300 m2/g)，1g汉生胶置于高速搅拌器中，搅拌速度为2000rpm，缓慢滴入60g的水，搅拌时间80min后，得到聚合物消泡剂，记为H。
对比例4
根据专利CN109929120A中实施例1制备，记为I。
消抑泡性能测试：
消泡剂性能对比测试方法如下
使用自配软木液，在循环鼓泡仪内测试样品A-样品I的消抑泡性能。将600mL 软木液注入循环鼓泡仪中内径为5cm 的硬质玻璃圆筒中，升温并维持在80℃，打开液体循环开关，控制流量至6L/min，当玻璃圆筒中泡沫高度上升至300mL 时，注入0.4mL 消泡剂并开始计时，同时记录泡沫高度，直至泡沫高度再次回升至300mL，停止液体循环。加入消泡剂后泡沫下降至250mL处的速度越快，最低泡沫高度越低，说明消泡性能越好；泡沫再次回升至300mL时所需时间越长说明消泡剂组合物抑泡性能越好。测试结果见表1。
表1. 消泡剂性能对比
数据表1，可以看出聚合物乳液型消泡剂样品A-样品E在造纸黑液测试中具有优异的消泡抑泡的效果，前期泡沫下降速率快，后期泡沫上升速度慢，样品F-样品I前期消泡速度较慢，同时后期泡沫回升速度快。
Claims (7)
1.一种聚合物乳液型消泡剂及其制备方法，其特征在于，所述的聚合物乳液消泡剂由以下组分组成：活性物占消泡剂总质量的10-35%，填料粒子占消泡剂总质量的3-8%，水占消泡剂总质量的60-85%，增稠剂占消泡剂总质量的0.5-3%；
一种聚合物乳液型消泡剂及其制备方法，所述活性物由丙烯酸酯，烯丙基聚醚，催化剂组成，其中丙烯酸酯占活性物总质量的29-70%，烯丙基聚醚占活性物总质量的29-70%，催化剂占活性物总质量的0.5-2%；
一种聚合物乳液型消泡剂及其制备方法，制备步骤如下：
（1）活性物的制备：将丙烯酸酯，催化剂加入烧瓶中，搅拌时间30-90min，将上述混合物滴入含有烯丙基聚醚的反应器中，反应温度60-100℃，滴加反应时间为2-8h；
（2）将活性物，填料粒子，增稠剂置于高速搅拌器中，搅拌速度为1500-2500rpm，缓慢滴入水，搅拌时间30-120min后，得到聚合物乳液消泡剂。
2.如权利要求1所述的一种聚合物乳液型消泡剂及其制备方法，其特征在于所述丙烯酸酯选自丙烯酸羟乙酯、丙烯酸甲酯、丙烯酸乙酯、丙烯酸丁酯、丙烯酸月桂酯、丙烯酸十八酯、丙烯酸异辛酯中的一种或两种以上任意比例混合。
3.如权利要求1所述的一种聚合物乳液型消泡剂及其制备方法，其特征在于，所述填料粒子选自疏水白炭黑、二氧化钛、氧化镁、氧化铝、乙二胺双硬脂酸酰胺(EBS)、硬脂酸铝中的一种或几种。
4.如权利要求3所述的一种聚合物乳液型消泡剂及其制备方法，其特征在于所述填料粒子比表面积为150～500m2/g。
5.如权利要求1所述的一种聚合物乳液型消泡剂及其制备方法，其特征在于，所述增稠剂为聚丙烯酰胺、卡波姆、汉生胶、聚丙烯酸酯、甲基纤维素、羧甲基纤维素、羟乙基纤维素、乙基纤维素中一种或几种。
6.如权利要求1所述的一种聚合物乳液型消泡剂及其制备方法，其特征在于，所述烯丙基聚醚的结构通式如下：CH2=CHCH2(OCH2CH2)a(OCH2CHCH3)b其中a为1-10整数，b为10-100整数。
7.如权利要求1所述的一种聚合物乳液型消泡剂及其制备方法，其特征在于，所述的的催化剂选自2,2’-偶氮双(2-甲基丙腈)，过氧化2-乙基己基酸叔丁酯，过氧化叔丁基，2,2’-偶氮双(2,4-二甲基戊腈)，2,2’-偶氮双(2-甲基丁腈)、过氧化苯甲酰中一种。
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| CN102649021A (zh) * | 2012-05-03 | 2012-08-29 | 安微銮威化工科技开发有限公司 | 一种非硅复合乳液型消泡剂及其制备方法 |
| US20170022327A1 (en) * | 2014-04-03 | 2017-01-26 | Dow Corning Toray Co., Ltd. | Novel silicone surfactant, w/o emulsion composition, powder composition, and cosmetic/medical application thereof |
| CN108786188A (zh) * | 2017-05-05 | 2018-11-13 | 江苏四新科技应用研究所股份有限公司 | 一种非硅消泡剂 |
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| DE102010009493A1 (de) * | 2010-02-26 | 2011-09-29 | Clariant International Limited | Polymere und ihre Verwendung als Dispergiermittel mit schaumhemmender Wirkung |
| JP5990667B2 (ja) * | 2011-10-24 | 2016-09-14 | サンノプコ株式会社 | 消泡剤 |
| JP6695760B2 (ja) * | 2015-08-19 | 2020-05-20 | Ｊｘｔｇエネルギー株式会社 | 消泡剤および潤滑油組成物 |
| CN110508037A (zh) * | 2019-08-29 | 2019-11-29 | 安徽銮威化工科技开发有限公司 | 一种非硅消泡剂及其制备装置 |
| CN111013201B (zh) * | 2019-12-03 | 2022-05-03 | 江苏四新科技应用研究所股份有限公司 | 消泡剂组合物 |
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| US20170022327A1 (en) * | 2014-04-03 | 2017-01-26 | Dow Corning Toray Co., Ltd. | Novel silicone surfactant, w/o emulsion composition, powder composition, and cosmetic/medical application thereof |
| CN108786188A (zh) * | 2017-05-05 | 2018-11-13 | 江苏四新科技应用研究所股份有限公司 | 一种非硅消泡剂 |
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