CN111484630A - Polymer emulsion type defoaming agent and preparation method thereof - Google Patents

Polymer emulsion type defoaming agent and preparation method thereof Download PDF

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Publication number
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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defoaming agent
acrylate
polymer emulsion
preparation
polymer
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李安宁
董飞
杨有忠
黄伟
曹添
安东尼·K·达西
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Nanjing Greenworld Research Institute Of New Materials Co ltd
Jiangsu Sixin Scientiric Technological Application Research Institute Co ltd
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Nanjing Greenworld Research Institute Of New Materials Co ltd
Jiangsu Sixin Scientiric Technological Application Research Institute Co ltd
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Priority to CN202010207349.8A priority Critical patent/CN111484630A/en
Priority to PCT/CN2020/081539 priority patent/WO2021189393A1/en
Publication of CN111484630A publication Critical patent/CN111484630A/en
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    • C—CHEMISTRY; METALLURGY
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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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    • B01D19/00—Degasification of liquids
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    • B01D19/04—Foam dispersion or prevention by addition of chemical substances
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    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C08K5/098—Metal salts of carboxylic acids
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    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/22—Expanded, porous or hollow particles
    • C08K7/24—Expanded, porous or hollow particles inorganic
    • C08K7/26—Silicon- containing compounds
    • 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
    • D21H21/06—Paper forming aids
    • D21H21/12—Defoamers
    • C—CHEMISTRY; METALLURGY
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    • 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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    • C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
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    • 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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    • 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
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    • C08K3/20—Oxides; Hydroxides
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Abstract

The invention provides a polymer emulsion type defoaming agent and a preparation method thereof, the components comprise an active substance, filler particles, water and a thickening agent, wherein the active substance consists of acrylic ester, allyl polyether and a catalyst, and the environmental protection problem caused by using harmful solvents such as toluene and the like in the traditional acrylic ester synthesis process is solved by introducing the allyl polyether containing a hydrophilic functional group into an acrylic ester polymer chain segment in the synthesis process; the double bond addition reaction forms a polymer macromolecule with self-emulsifying function, which can be emulsified in water to form emulsions with different particle size ranges; the polymer emulsion can realize self-emulsification to form emulsion, so that a series of problems of floating oil precipitation, emulsion breaking and the like caused by using some emulsifiers in the traditional organosilicon emulsion type defoaming agent are solved.

Description

Polymer emulsion type defoaming agent and preparation method thereof
Technical Field
The invention relates to a polymer emulsion type defoaming agent and a preparation method thereof, wherein the polymer emulsion is an important fine chemical additive, and therefore, the invention belongs to the technical field of fine chemical preparations.
Background
Paper making is a key industry in national economic production. In the paper industry, a variety of surfactants, such as defoamers, are commonly used. Most industrial processes involve considerable hazards, such as reduced machine efficiency, delayed working time, and the quality of the final product. The method for eliminating harmful foam generally adopts a mode of adding a defoaming agent. The defoaming agent is divided into non-silicon type and organic silicon type. Compared with other defoaming agents, the organic silicon defoaming agent has the advantages of stable chemical property, stable chemical resistance and small side effect, and has good instant defoaming capability under the condition of low dosage, so that the organic silicon defoaming agent is favored. The non-silicon defoaming agent takes mineral oil, polyether, amide or fatty alcohol, acrylate as active substances, and when a large amount of the non-silicon defoaming agent is used, the active substances, namely amide, can gradually aggregate and coagulate, and spots are remained on paper; and the mineral oil can generate tetrachlorodibenzo-p-dioxin (TCDD) harmful substances under the condition of long-time high temperature, thus harming the personal safety and the environmental safety. The organic silicon defoaming agent takes polysiloxane, filler and the like as active substances, and long-time use of the organic silicon defoaming agent can cause the agglomeration of hydrophobic particles, and the hydrophobic particles are attached to paper to form silicon spots, so that the quality of the paper is reduced.
Patent US5152925A describes a defoaming agent using polyacrylate as a main defoaming active substance, wherein the acrylate polymer mainly uses an acrylate polymer prepared by using hydroxyl-containing acrylate monomer in solvents such as diisodecyl phthalate (DIDP) or DIOP as a main active substance, and is applied to black liquor washing and other papermaking processes. Patent CN102428142B also mentions that acrylate polymer is used as an active substance to prepare a bulk defoaming agent, wherein the acrylate polymer is prepared from monomers such as isooctyl acrylate, hydroxy acrylate and acrylic acid in polybutene or polyether solvent, and the prepared acrylate polymer is used as a main active ingredient of the defoaming agent and is compounded with defoaming aids such as white carbon black and alkyl silicone oil, and is applied to industries such as petroleum exploitation, water treatment, coating industry and ink, food and beverage processing, drilling industry, textile industry, paper making and the like. The defoaming agent can solve the problem of silicon precipitation residue of the traditional organic silicon defoaming agent, but the defoaming and foam inhibiting performance of the defoaming agent prepared by the prior art still has a great space for improvement. Therefore, the improvement of the defoaming and foam inhibiting performance of the acrylate polymer defoaming agent is of great significance.
Disclosure of Invention
The invention solves the existing problems and provides an emulsion type defoaming agent based on a polymer as an active substance. The advantages of the invention are as follows:
(1) the polymer with self-emulsifying function is formed by introducing allyl polyether containing hydrophilic functional groups into an acrylate polymer chain segment and performing double bond addition reaction, the molecular weight is adjusted by the content of a catalyst and the reaction time to have certain viscosity, and the polymer can be emulsified in water to form emulsions with different particle size ranges.
(2) Allyl polyether introduced into high molecular polymer, and its structure (OCH)2CH2)aAnd (OCH)2CHCH3)bAdjusting the hydrophilic-hydrophobic balance value (H L B), (OCH)2CH2)aThe increase can obviously improve the hydrophilic performance, (OCH)2CHCH3)bThe hydrophobic properties can be adjusted to achieve self-emulsification of the molecular structure to form an emulsion.
(3) In the synthesis process, the allyl polyether has low viscosity, not only serves as a reaction monomer, but also realizes the function of a reaction solvent, and solves the environmental protection problem caused by using harmful solvents such as toluene and the like in the traditional acrylate synthesis process.
(4) The polymer emulsion can realize self-emulsification to form emulsion, so that a series of problems of floating oil precipitation, emulsion breaking and the like caused by using some emulsifiers in the traditional organosilicon emulsion type defoaming agent are solved.
In order to realize the effect, the technical scheme of the polymer emulsion type defoaming agent and the preparation method is as follows:
a polymer emulsion type defoaming agent comprises the following components: the active matter accounts for 10-35% of the total mass of the defoaming agent, the filler particles accounts for 3-8% of the total mass of the defoaming agent, the water accounts for 60-85% of the total mass of the defoaming agent, and the thickening agent accounts for 0.5-3% of the total mass of the defoaming agent;
the polymer emulsion type defoaming agent comprises an active matter, allyl polyether and a catalyst, wherein the active matter comprises 29-70% of acrylate, 29-70% of allyl polyether and 0.5-2% of catalyst, wherein the acrylate accounts for the total mass of the active matter;
a polymer latex type defoaming agent and its preparation method, said acrylate is selected from hydroxy ethyl acrylate, methyl acrylate, ethyl acrylate, butyl acrylate, lauryl acrylate, octadecyl acrylate, iso octyl acrylate one or more than two of any proportion to mix;
a polymer emulsion type defoaming agent and a preparation method thereof, wherein filler particles are selected from one or more of hydrophobic white carbon black, titanium dioxide, magnesium oxide, aluminum oxide, Ethylenediamine Bisstearamide (EBS) and aluminum stearate;
polymer emulsion type defoaming agent and preparation method thereof, wherein the specific surface area of the filler particles is 150-500 m2/g；
The polymer emulsion type defoaming agent and the preparation method thereof are characterized in that the thickening agent is one or more of polyacrylamide, carbomer, xanthan gum, polyacrylate, methyl cellulose, carboxymethyl cellulose, hydroxyethyl cellulose and ethyl cellulose;
a polymer emulsion type defoaming agent and a preparation method thereof are disclosed, wherein the general structural formula of the allyl polyether is as follows:
CH2=CHCH2(OCH2CH2)a(OCH2CHCH3)bwherein a is an integer of 1 to 10 and b is an integer of 10 to 100.
A polymer emulsion type defoaming agent and a preparation method thereof, wherein the catalyst is selected from one of 2,2 ' -azobis (2-methyl propionitrile), tert-butyl 2-ethylhexyl peroxide, tert-butyl peroxide, 2,2 ' -azobis (2, 4-dimethyl valeronitrile), 2,2 ' -azobis (2-methyl butyronitrile) and benzoyl peroxide;
a preparation method of a polymer emulsion type defoaming agent comprises the following steps:
(1) preparation of active matter: adding acrylate and a catalyst into a flask, stirring for 30-90min, dripping the mixture into a reactor containing allyl polyether, wherein the reaction temperature is 60-100 ℃, and the dripping reaction time is 2-8 h;
(2) and (3) placing the active substance, the filler particles and the thickening agent into a high-speed stirrer at the stirring speed of 1500-2500rpm, slowly dripping water, and stirring for 30-120min to obtain the polymer emulsion defoaming agent.
Detailed Description
The first embodiment,
(1) Preparation of active matter: adding hydroxyethyl acrylate 10g, isooctyl acrylate 19g, and catalyst 2, 2' -azobis (2-methylpropanenitrile) 1g into a flask, stirring for 30min, and adding dropwise the mixture containing allyl polyether CH 70g2=CHCH2(OCH2CH2)(OCH2CHCH3)100The reaction temperature in the reactor is 60 ℃, and the dropwise adding reaction time is 8 hours;
(2) 10g of active substance and 8g of hydrophobic white carbon black (the specific surface area is 150 m)2And/g), 1g of polyacrylamide and 2g of polyacrylate are placed in a high-speed stirrer, the stirring speed is 1500rpm, 79g of water is slowly dropped into the stirrer, and after the stirring time is 120min, the polymer emulsion defoaming agent is obtained and is marked as A.
Example II,
(1) Preparation of active matter: 70g of ethyl acrylate and 1g of the catalyst tert-butyl 2-ethylhexyl peroxide are added to the flask, the mixture is stirred for 90min, and the mixture is added dropwise to a flask containing 29g of allyl polyether CH2=CHCH2(OCH2CH2)10(OCH2CHCH3)10The reaction temperature in the reactor is 100 ℃, and the dropwise reaction time is 2 hours;
(2) 35g of active substance, 3g of titanium dioxide (specific surface area 300 m)2And/g), 0.5g of polyacrylamide is placed in a high-speed stirrer, the stirring speed is 2500rpm, 61.5g of water is slowly dropped, and after stirring for 30min, a polymer emulsion defoaming agent is obtained, which is recorded as B.
Example III,
(1) Preparation of active matter: adding 10g of lauryl acrylate, 35g of butyl acrylate and 0.5g of benzoyl peroxide as a catalyst into a flask, stirring for 60min, and dropwise adding the mixture containing 54.5g of allyl polyether CH2=CHCH2(OCH2CH2)5(OCH2CHCH3)50The reaction temperature in the reactor is 80 ℃, and the dropwise reaction time is 5 hours;
(2) 34g of active substance, 2g of ethylenediamine bisstearamide (specific surface area 200 m)2Per g), 3g stearinAluminium acid (specific surface area 300 m)2And/g), 1g of xanthan gum is placed in a high-speed stirrer, the stirring speed is 2000rpm, 60g of water is slowly dropped, and after the stirring time is 80min, the polymer emulsion defoaming agent is obtained, and is marked as C.
Example four,
(1) Preparation of active matter: adding 60g methyl acrylate, 5g octadecyl acrylate, 2g catalyst 2, 2' -azobis (2-methylbutyronitrile) into flask, stirring for 50min, and adding dropwise the above mixture containing 33g allyl polyether CH2=CHCH2(OCH2CH2)8(OCH2CHCH3)65The reaction temperature in the reactor is 70 ℃, and the dropwise reaction time is 4 hours;
(2) 10.5g of active, 1.5g of carbomer, 1.5g of magnesium oxide (specific surface area 250 m)2Per gram), 1.5g of alumina (specific surface area 300 m)2And/g) is placed in a high-speed stirrer, the stirring speed is 2300rpm, 85g of water is slowly dropped into the stirrer, and after the stirring time is 100min, the polymer emulsion defoaming agent is obtained and is marked as D.
Example V,
(1) Preparation of active matter: adding hydroxyethyl acrylate 10g, isooctyl acrylate 10g, butyl acrylate 10g, tert-butyl peroxide 1.5g into flask, stirring for 40min, and adding the above mixture dropwise to a solution containing allyl polyether CH 48.5g2=CHCH2(OCH2CH2)3(OCH2CHCH3)32The reaction temperature in the reactor is 70 ℃, and the dropwise reaction time is 7 hours;
(2) 22g of active substance, 6g of aluminum stearate (specific surface area 350 m)2And/g), 2g of carboxymethyl cellulose is placed in a high-speed stirrer, the stirring speed is 1600rpm, 70g of water is slowly dropped into the stirrer, and after the stirring time is 50min, the polymer emulsion defoaming agent is obtained and is marked as E.
Comparative example 1
(1) Preparation of active matter: adding 40g of hydroxyethyl acrylate, 58g of isooctyl acrylate and 2g of catalyst 2, 2' -azobis (2-methyl propionitrile) into a flask, uniformly stirring, heating to the reaction temperature of 60 ℃, and reacting for 8 hours;
(2) 10g of active substance and 8g of hydrophobic white carbon black (the specific surface area is 150 m)2And/g), 1g of polyacrylamide and 2g of polyacrylate are placed in a high-speed stirrer, the stirring speed is 1500rpm, 79g of water is slowly dropped into the stirrer, and after the stirring time is 120min, the polymer defoaming agent is obtained and is marked as F.
Comparative example 2
(1) Preparation of active matter: 70g of ethyl acrylate and 1g of the catalyst tert-butyl 2-ethylhexyl peroxide are added to the flask, the mixture is stirred for 90min, and the mixture is added dropwise to a flask containing 29g of allyl polyether CH2=CHCH2(OCH2CH2)100(OCH2CHCH3)200The reaction temperature in the reactor is 100 ℃, and the dropwise reaction time is 2 hours;
(2) 35g of active substance, 3g of titanium dioxide (specific surface area 300 m)2/G), 0.5G of polyacrylamide was placed in a high-speed stirrer at 2500rpm, 61.5G of water were slowly added dropwise thereto, and after stirring for 30min, a polymer defoamer, denoted as G, was obtained.
Comparative example 3
(1) Preparation of active matter: adding 10g of lauryl acrylate, 35g of butyl acrylate and 0.5g of benzoyl peroxide as a catalyst into a flask, stirring for 60min, and dropwise adding the mixture containing 54.5g of allyl polyether CH2=CHCH2(OCH2CH2)5(OCH2CHCH3)3The reaction temperature in the reactor is 80 ℃, and the dropwise reaction time is 5 hours;
(2) 34g of active substance, 2g of ethylenediamine bisstearamide (specific surface area 200 m)2Per g), 3g of aluminum stearate (specific surface area 300 m)2And/g), 1g of xanthan gum is placed in a high-speed stirrer, the stirring speed is 2000rpm, 60g of water is slowly dropped, and after the stirring time is 80min, a polymer antifoaming agent is obtained, and is recorded as H.
Comparative example 4
Prepared according to patent CN109929120A, example 1, noted I.
And (3) testing defoaming and foam inhibiting performance:
the comparative testing method of the performance of the defoaming agent is as follows
The defoaming performance of the sample A-sample I is tested in a circulating bubbler by using self-prepared cork liquid, 600m L cork liquid is injected into a hard glass cylinder with the inner diameter of 5cm in the circulating bubbler, the temperature is raised and maintained at 80 ℃, a liquid circulating switch is opened, the flow rate is controlled to be 6L/min, when the foam height in the glass cylinder rises to 300m L, 0.4m L defoaming agent is injected and timing is started, the foam height is recorded at the same time until the foam height rises to 300m L again, the liquid circulation is stopped, the speed of the foam falling to 250m L after the defoaming agent is added is faster, the lowest foam height is lower, the better the defoaming performance is indicated, the longer the time required for the foam to rise to 300m L again is longer, the better the defoaming performance is indicated, and the test results are shown in Table 1.
TABLE 1 comparison of defoamer Properties
Figure DEST_PATH_IMAGE001
Data table 1 shows that polymer emulsion type defoaming agent samples a to E have excellent defoaming and foam-suppressing effects in the papermaking black liquor test, the foam descending speed in the early stage is high, the foam ascending speed in the later stage is low, the defoaming speed in the early stage of samples F to I is low, and the foam rising speed in the later stage is high.

Claims (7)

1. The polymer emulsion type defoaming agent is characterized by comprising the following components in parts by weight: the active matter accounts for 10-35% of the total mass of the defoaming agent, the filler particles accounts for 3-8% of the total mass of the defoaming agent, the water accounts for 60-85% of the total mass of the defoaming agent, and the thickening agent accounts for 0.5-3% of the total mass of the defoaming agent;
the polymer emulsion type defoaming agent comprises an active matter, allyl polyether and a catalyst, wherein the active matter comprises 29-70% of acrylate, 29-70% of allyl polyether and 0.5-2% of catalyst, wherein the acrylate accounts for the total mass of the active matter;
a polymer emulsion type defoaming agent and a preparation method thereof comprise the following preparation steps:
(1) preparation of active matter: adding acrylate and a catalyst into a flask, stirring for 30-90min, dripping the mixture into a reactor containing allyl polyether, wherein the reaction temperature is 60-100 ℃, and the dripping reaction time is 2-8 h;
(2) and (3) placing the active substance, the filler particles and the thickening agent into a high-speed stirrer at the stirring speed of 1500-2500rpm, slowly dripping water, and stirring for 30-120min to obtain the polymer emulsion defoaming agent.
2. A polymer emulsion defoaming agent as claimed in claim 1 wherein said acrylate is selected from the group consisting of hydroxyethyl acrylate, methyl acrylate, ethyl acrylate, butyl acrylate, lauryl acrylate, stearyl acrylate and isooctyl acrylate, and is mixed in any proportion.
3. The polymer emulsion defoaming agent according to claim 1 and its preparation method, wherein said filler particles are selected from one or more of hydrophobic white carbon black, titanium dioxide, magnesium oxide, aluminum oxide, Ethylenediamine Bisstearamide (EBS), and aluminum stearate.
4. The polymer emulsion-type defoaming agent according to claim 3 wherein the specific surface area of the filler particles is 150 to 500m 2/g.
5. The polymeric emulsion defoaming agent according to claim 1, wherein said thickener is one or more selected from the group consisting of polyacrylamide, carbomer, xanthan gum, polyacrylate, methyl cellulose, carboxymethyl cellulose, hydroxyethyl cellulose and ethyl cellulose.
6. The polymeric emulsion defoamer as claimed in claim 1, wherein said allyl polyether has the following general structural formula: CH2= CHCH2(OCH2CH2) a (OCH2CHCH3) b wherein a is an integer from 1 to 10 and b is an integer from 10 to 100.
7. A polymer emulsion defoaming agent and a preparation method thereof as claimed in claim 1 wherein said catalyst is selected from one of 2,2 ' -azobis (2-methylpropanenitrile), tert-butyl peroxy-2-ethylhexyl, tert-butyl peroxide, 2,2 ' -azobis (2, 4-dimethylvaleronitrile), 2,2 ' -azobis (2-methylbutyronitrile) and benzoyl peroxide.
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