CN106905474B - A kind of sealing composite pad aqueous high molecular composite emulsion and preparation process - Google Patents
A kind of sealing composite pad aqueous high molecular composite emulsion and preparation process Download PDFInfo
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- CN106905474B CN106905474B CN201710029802.9A CN201710029802A CN106905474B CN 106905474 B CN106905474 B CN 106905474B CN 201710029802 A CN201710029802 A CN 201710029802A CN 106905474 B CN106905474 B CN 106905474B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—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 a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
-
- 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
- D21H19/00—Coated paper; Coating material
- D21H19/10—Coatings without pigments
- D21H19/14—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12
- D21H19/20—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12 comprising macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- D21H21/14—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 characterised by function or properties in or on the paper
- D21H21/16—Sizing or water-repelling agents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—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 a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
Abstract
The invention discloses a kind of sealing composite pad aqueous high molecular composite emulsions, are made of following weight parts raw material: butyl acrylate 80 ~ 100, methyl methacrylate 30 ~ 40, acrylonitrile 28 ~ 42, styrene 16 ~ 20, acrylic acid 3 ~ 6, water 442 ~ 490, triethanolamine 2 ~ 6, phenoxetol 0.1-1, emulsifier 2 ~ 6, crosslinking agent 4 ~ 8, initiator 0.1 ~ 1, the present invention discloses the preparation processes of the composite emulsion.A kind of sealing composite pad aqueous high molecular composite emulsion provided by the invention, reaction process Environmental Safety, solvent-free volatilization is reacted under water-based system, also without waste water, discarded discharge, non-stimulated smell, harm to the human body are small in use process, in the use process of mechanical Special seal composite pad, make gasket bonding itself securely, good seal performance, long service life, waste paper can be made to recycle simultaneously, reach environmental protection and energy saving effect.
Description
Technical field
The invention belongs to new material technology fields, and in particular to a kind of sealing composite pad aqueous high molecular composite emulsion and
Preparation process.
Background technique
Esters of acrylic acid product characteristic is excellent, is widely used in the row such as coating, adhesive, leather, chemical fibre, papermaking, printing
Industry, wherein may be utilized in fabricating adhesive tape, sponge oil resistant gasket, adhesive of medical etc., aviation, rocket, guided missile in adhesive industry
Etc. hard-core technologies department be used for preparing the adhesive of solid fuel.
Patent 201510308478.5 discloses acroleic acid binding agent and preparation method thereof, and the adhesion strength of the invention is stronger
And microhardness is moderate.
Patent 201410730559.X discloses a kind of leather finishing agent, suitable for the covering with paint of various leathers, after covering with paint
Leather soft glossy naturally, good hand feeling moisten, the rub resistance ability of leather surface can be improved, but do not mention the product and exist
Binder aspect and the application in automobile sealed accessory.
Patent 201210074122.6 discloses a kind of fire-retardant polyacrylacid ester latex and preparation method thereof, this method institute
Latex has excellent anti-flammability, adhesiveness, at model and stability and splendid water resistance, can be widely used for adhesive,
The industries such as coating have water resistance.
Since esters of acrylic acid product has superior resistance to mineral oil and pyro-oxidation resistance, keep it close in all kinds of automobiles
Envelope accessory has comparative advantage.Acrylate can be developed into aqueous high molecular compounded latex through scientific matching optimization.
Big 26 resin of butylene of the smell of many decades of composite pad industrial application at present, toxicity, there are caused by many defects
Problem.
Summary of the invention
To solve the above problems, the present invention provides a kind of sealing composite pad aqueous high molecular composite emulsion, the Composite Milk
Glue smell is small, and environmentally friendly and cohesive force is strong.
A kind of sealing composite pad aqueous high molecular composite emulsion, is made of following weight parts raw material: butyl acrylate 80 ~
100, methyl methacrylate 30 ~ 40, acrylonitrile 28 ~ 42, styrene 16 ~ 20, acrylic acid 3 ~ 6, water 442 ~ 490, triethanolamine 2
~ 6, phenoxetol 0.1-1, emulsifier 2 ~ 6, crosslinking agent 4 ~ 8, initiator 0.1 ~ 1.
Preferably, the emulsifier is selected from alkyl phenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, polyoxyethylene wool
It is two or more in alcohol ether, polyoxyethylene cholesterol's ether, lauryl sodium sulfate, stearoyl lactate and stearyl lactate.
Preferably, the initiator is selected from one or more of ammonium persulfate, potassium peroxydisulfate and sodium peroxydisulfate.
Preferably, the crosslinking agent is selected from ethylene glycol dimethacrylate, N hydroxymethyl acrylamide and divinyl
One or more of base benzene.
The preparation process of composite emulsion described above, comprising the following steps:
(1) by reaction monomers butyl acrylate, methyl methacrylate, acrylonitrile, styrene, acrylic acid and phenoxy group second
Alcohol is uniformly mixed according to mass ratio；
(2) deionized water and emulsifier are added in reaction kettle, while being added 1/3 of reaction monomers total amount in step (1), rises
Temperature；
(3) when temperature reaches 62 DEG C, step (1) residual monomer, initiator and crosslinking agent control time for adding are added anti-
Kettle is answered, control temperature of reaction system is 86-88 DEG C during being added dropwise；
(4) after being added dropwise to complete, control system stablizes 75-85 DEG C, keeps the temperature 1.5-3 hours, and after heat preservation, three ethyl alcohol are added
Amine adjusts pH value, and is cooled to 40-50 DEG C, obtains multiple emulsion.
Preferably, when reaction monomers in step (1) being added in the step (2), control mixing speed is 80-100r/
Min, heating rate are 1-2 DEG C/min.
Preferably, control time for adding is 1.5-2.5 hours in the step (3), and mixing speed at this time is 90-
110r/min。
Preferably, in the step (4) during heat preservation, the mixing speed of control system is 100-120 r/min.
The molecular weight for the multiple emulsion that above-mentioned preparation process obtains is 100000-200000 dalton, solid content 27-
31%, viscosity 500-5000cp.s.
The present invention discloses application of the composite emulsion in mechanical Special seal composite pad.
Composite emulsion use process is that latex is added in paper pulp, other effective component compression mouldings with gasket.
For the present invention during preparing composite emulsion, the ratio of various monomers wants strict control, is more than and is less than not
Multiple emulsion of good performance can be prepared.It is mechanical dedicated close that composite emulsion of the invention is applied to gasoline engine or diesel engine etc.
When packing, good seal performance, suitable for being used in the various atrocious weathers such as high temperature and low temperature.
Beneficial effect
A kind of sealing composite pad aqueous high molecular composite emulsion provided by the invention, reaction process Environmental Safety are aqueous
Solvent-free volatilization is reacted under system, also without waste water, discarded discharge, non-stimulated smell, harm to the human body in use process
It is small, in the use process of mechanical Special seal composite pad, make gasket bonding itself securely, good seal performance, service life
It is long, while waste paper can be made to recycle, reach environmental protection and energy saving effect.
Embodiment
Embodiment 1
(1) a kind of sealing composite pad aqueous high molecular composite emulsion is formed by following raw materials: butyl acrylate 80Kg,
Methyl methacrylate 30Kg, acrylonitrile 28Kg, styrene 16Kg, acrylic acid 3Kg and phenoxetol 0.1Kg are configured to anti-
Answer monomer.
(2) 442 Kg of deionized water, fatty alcohol polyoxyethylene ether 1Kg, stearoyl lactate 1Kg, hard is added in reaction kettle
Acyl calcium lactate 1Kg and polyoxyethylene wool alcohol ether 1Kg, forms excellent aqueous reaction system.In the aqueous reaction system,
It is added the 1/3 of reaction monomers total amount, reaction system is made to heat up.At this time control mixing speed be 80r/min, heating rate be 1 DEG C/
min。
(3) when reaction system reaches 62 DEG C, remaining reaction monomers are added dropwise in the reaction system, while over cure is added
Sour ammonium 0.02Kg, potassium peroxydisulfate 0.05Kg and sodium peroxydisulfate 0.03Kg, 1 Kg, N- methylol third of ethylene glycol dimethacrylate
1 Kg of acrylamide and divinylbenzene 2Kg, drips for 1.5 hours, and mixing speed at this time is 90r/min.Make reacting balance into
Row forms high molecular crosslink elastic net structure, controls temperature of reaction system at 86 DEG C.
(4) after being added dropwise to complete, control system stablizes 75 DEG C, keeps the temperature 1.5 hours, during heat preservation, control system is stirred
Mixing speed is 100r/min.After heat preservation, it is 9 that triethanolamine 2kg, which is added, and adjusts pH value, and is cooled to 50 DEG C, is obtained compound
Lotion, system are translucent, with blue light, milky water-based emulsion.
Embodiment 2
(1) a kind of sealing composite pad aqueous high molecular composite emulsion is formed by following raw materials: butyl acrylate 100Kg,
Methyl methacrylate 40 Kg, acrylonitrile 42Kg, 20 Kg of styrene, acrylic acid 6 Kg and phenoxetol 1Kg are configured to lead
Want reaction monomers.
(2) 490 Kg of deionized water, polyoxyethylene wool alcohol ether 1Kg, fatty alcohol polyoxyethylene ether are added in reaction kettle
1Kg, stearoyl lactate 3Kg and stearyl lactate 1Kg form excellent aqueous reaction system.In the aqueous reaction system
In, the 1/3 of reaction monomers total amount is added, reaction system is made to heat up.Control mixing speed is 100r/min at this time, and heating rate is
2℃/min。
(3) when reaction system reaches 60 DEG C, remaining reaction monomers are added dropwise in the reaction system, while over cure is added
Sour ammonium 0.5Kg, potassium peroxydisulfate 0.5Kg, 4 Kg of ethylene glycol dimethacrylate and divinylbenzene 4Kg, are added dropwise for 2.5 hours
Complete, mixing speed at this time is 110r/min.Reacting balance is carried out, high molecular crosslink elastic net structure is formed, control is anti-
Answer system temperature at 88 DEG C.
(4) after being added dropwise to complete, control system stablizes 85 DEG C, keeps the temperature 3 hours, during heat preservation, the stirring of control system
Speed is 120 r/min.After heat preservation, it is 10 that triethanolamine 6kg, which is added, and adjusts pH value, and is cooled to 40 DEG C, is obtained compound
Lotion, system are translucent, with blue light, milky water-based emulsion.
Embodiment 3
(1) a kind of sealing composite pad aqueous high molecular composite emulsion is formed by following raw materials: butyl acrylate 90Kg,
Methyl methacrylate 35 Kg, acrylonitrile 36Kg, 18 Kg of styrene, acrylic acid 4 Kg and phenoxetol 0.5Kg are configured to
Key reaction monomer.
(2) 465 Kg of deionized water, 0.5 Kg of polyoxyethylene wool alcohol ether, polyoxyethylene cholesterol's ether are added in reaction kettle
1 Kg, stearoyl lactate 2Kg and stearyl lactate 0.5Kg form excellent aqueous reaction system.In the aqueous reactant
In system, the one third of reaction monomers total amount is added, reaction system is made to heat up.Control mixing speed is 90r/min, heating at this time
Rate is 2 DEG C/min.
(3) when reaction system reaches 60 DEG C, remaining reaction monomers are added dropwise in the reaction system, while over cure is added
Sour sodium 0.1Kg, potassium peroxydisulfate 0.35Kg, 1 Kg of N hydroxymethyl acrylamide and divinylbenzene 5Kg, drip, at this time for 2 hours
Mixing speed be 100r/min.Reacting balance is carried out, high molecular crosslink elastic net structure is formed, controls reaction system temperature
Degree is at 87 DEG C.
(4) after being added dropwise to complete, control system stablizes 80 DEG C, keeps the temperature 2.5 hours, during heat preservation, control system is stirred
Mixing speed is 110r/min.After heat preservation, it is 9.5 that triethanolamine 4kg, which is added, and adjusts pH value, and is cooled to 45 DEG C, is answered
Lotion is closed, system is translucent, with blue light, milky water-based emulsion.
Comparative example 1
(1) a kind of sealing composite pad aqueous high molecular composite emulsion, by following raw materials form: by quantitative water, monomer,
Reaction kettle is added in emulsifier and crosslinking agent together, 15-40 DEG C at a temperature of, stirring, wherein 620 Kg of water, monomer: acrylic acid
7 Kg, butyl acrylate 200Kg, 40 Kg of ethyl acrylate, styrene 50Kg, 30 Kg of methyl methacrylate, acrylonitrile
20Kg；3 Kg of emulsifier sodium lauryl sulfate, isomeric alcohol polyethenoxy ether 4Kg and peregal 15Kg；Crosslinking agent includes N- hydroxyl
Methacrylamide 5kg and itaconic acid 6kg.
(2) ammonium persulfate 0.45Kg, potassium peroxydisulfate 0.28Kg are added, is stirred.
(3) reducing agent is added and stabilizer continues to stir, heat up, until 70-75 DEG C；Reducing agent is the 0.3% of monomer gross mass
Green vitriol and monomer gross mass 0.4% sodium hydrogensulfite, stabilizer be monomer gross mass 1% triethanolamine
With the 0.05% of monomer gross mass sodium bicarbonate.
(4) 0.04% hydrogen peroxide of above-mentioned monomer gross mass and the tert-butyl hydroperoxide of monomer gross mass 0.02% are added
Hydrogen keeps the temperature 1.5 hours, cooling, adjusts pH value 6.8-7 with ammonium hydroxide, obtains finished product.
Comparative example 2
(1) a kind of sealing composite pad aqueous high molecular composite emulsion is formed by following raw materials: butyl acrylate 90Kg,
Methyl methacrylate 35 Kg, acrylonitrile 36Kg, 18 Kg of styrene, acrylic acid 4 Kg and phenoxetol 0.5Kg are configured to
Key reaction monomer.
(2) 350 Kg of deionized water is added in reaction kettle, 5 Kg of polyoxyethylene cholesterol's ether forms excellent aqueous reaction
System.In the aqueous reaction system, the one third of reaction monomers total amount is added, reaction system is made to heat up.Control is stirred at this time
Mixing speed is 70r/min, and heating rate is 5 DEG C/min.
(3) when reaction system reaches 60 DEG C, remaining reaction monomers are added dropwise in the reaction system, while over cure is added
Sour potassium 0.5Kg, N hydroxymethyl acrylamide 6Kg, drip for 1 hour, control temperature of reaction system at 80 DEG C.Triethanolamine is added
It is 9.5 that 4kg, which adjusts pH value,
(4) after being added dropwise to complete, control system stablizes 90 DEG C, keeps the temperature 2.5 hours, during heat preservation, control system is stirred
Mixing speed is 70r/min.45 DEG C are cooled to, water-based emulsion is obtained.
Water resistant, oil resistant and surface strength variation before and after 2 body paper top sizing of table
Old paper stock is added in the lotion of embodiment and comparative example preparation, is pressed into together with the other compositions of gasket
Type, the performance test under the same terms are as follows:
Water-fast and oil resistant performance test is as follows:
Claims (9)
1. a kind of sealing composite pad aqueous high molecular composite emulsion, which is characterized in that be made of following weight parts raw material: propylene
Acid butyl ester 80 ~ 100, methyl methacrylate 30 ~ 40, acrylonitrile 28 ~ 42, styrene 16 ~ 20, acrylic acid 3 ~ 6, water 442 ~ 490,
Triethanolamine 2 ~ 6, phenoxetol 0.1-1, emulsifier 2 ~ 6, crosslinking agent 4 ~ 8, initiator 0.1 ~ 1；
The emulsifier are as follows: polyoxyethylene wool alcohol ether, fatty alcohol polyoxyethylene ether, stearoyl lactate, stearoyl lactylates
The mass ratio of calcium is 1:1:1:1 or 1:1:3:1.
2. composite emulsion according to claim 1, which is characterized in that the initiator is selected from ammonium persulfate, persulfuric acid
One or more of potassium and sodium peroxydisulfate.
3. composite emulsion according to claim 1, which is characterized in that the crosslinking agent is selected from dimethacrylate second two
One or more of alcohol ester, N hydroxymethyl acrylamide and divinylbenzene.
4. a kind of preparation process of composite emulsion as described in any one of claims 1-3, which is characterized in that including following step
It is rapid:
(1) reaction monomers butyl acrylate, methyl methacrylate, acrylonitrile, styrene, acrylic acid and phenoxetol are pressed
It is uniformly mixed according to mass ratio；
(2) deionized water and emulsifier are added in reaction kettle, while being added 1/3 of reaction monomers total amount in step (1), heats up；
(3) when temperature reaches 62 DEG C, reaction kettle is added in step (1) residual monomer, initiator and crosslinking agent control time for adding,
Control temperature of reaction system is 86-88 DEG C during being added dropwise；
(4) after being added dropwise to complete, control system stablizes 75-85 DEG C, keeps the temperature 1.5-3 hours, and after heat preservation, triethanolamine tune is added
PH value is saved, and is cooled to 40-50 DEG C, obtains multiple emulsion.
5. preparation process according to claim 4, which is characterized in that it is single that reaction in step (1) is added in the step (2)
When body, control mixing speed is 80-100r/min, and heating rate is 1-2 DEG C/min.
6. preparation process according to claim 4, which is characterized in that control time for adding is 1.5- in the step (3)
2.5 hours, mixing speed at this time was 90-110r/min.
7. preparation process according to claim 4, which is characterized in that in the step (4) during heat preservation, control volume
The mixing speed of system is 100-120 r/min.
8. preparation process according to claim 4, which is characterized in that the molecular weight of obtained multiple emulsion is 100000-
200000 dalton, solid content 27-31%, viscosity 500-5000cp.s.
9. a kind of application of composite emulsion as described in one of claim 1-3 in mechanical Special seal composite pad.
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| CN109749027A (en) * | 2017-11-05 | 2019-05-14 | 丹阳市贝尔特橡塑制品有限公司 | A kind of gasket of good airproof performance |
| CN110791234A (en) * | 2019-10-30 | 2020-02-14 | 广州全系建材有限公司 | Continuous-bonding ceramic tile adhesive and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101704913A (en) * | 2009-09-29 | 2010-05-12 | 上海东升新材料有限公司 | Styrene-acrylic emulsion for priming paint as well as preparation method and application thereof |
| CN102757522A (en) * | 2011-04-25 | 2012-10-31 | 北京化工大学 | Synthetic method of anionic surface sizing agent |
| CN105713131A (en) * | 2014-12-04 | 2016-06-29 | 上海东升新材料有限公司 | Styrene-acrylic emulsion, preparation method and application thereof |
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2017
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101704913A (en) * | 2009-09-29 | 2010-05-12 | 上海东升新材料有限公司 | Styrene-acrylic emulsion for priming paint as well as preparation method and application thereof |
| CN102757522A (en) * | 2011-04-25 | 2012-10-31 | 北京化工大学 | Synthetic method of anionic surface sizing agent |
| CN105713131A (en) * | 2014-12-04 | 2016-06-29 | 上海东升新材料有限公司 | Styrene-acrylic emulsion, preparation method and application thereof |
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