CN111154020A - Regenerated carboxylic styrene-butadiene latex for leather and preparation method thereof - Google Patents
Regenerated carboxylic styrene-butadiene latex for leather and preparation method thereof Download PDFInfo
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- CN111154020A CN111154020A CN202010060721.7A CN202010060721A CN111154020A CN 111154020 A CN111154020 A CN 111154020A CN 202010060721 A CN202010060721 A CN 202010060721A CN 111154020 A CN111154020 A CN 111154020A
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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
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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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
- 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
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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
- C08F236/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds
- C08F236/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds
- C08F236/04—Copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds conjugated
- C08F236/10—Copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds conjugated with vinyl-aromatic monomers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J113/00—Adhesives based on rubbers containing carboxyl groups
- C09J113/02—Latex
Abstract
The invention discloses a regenerated carboxylic styrene-butadiene latex for leather and a preparation method thereof. The carboxylic styrene-butadiene latex comprises the following components in parts by weight: 100 parts of main monomer; 80-110 parts of water; 2-4 parts of a functional monomer; 2-3 parts of auxiliary monomer; 0.7-1.2 parts of an initiator; 1-2 parts of a crosslinking agent; 2-3.5 parts of an emulsifier; 3-6 parts of an antioxidant; the main monomer consists of 50-60% of styrene and the balance of butadiene; the functional monomer is composed of at least one of itaconic acid, acrylic acid, methacrylic acid and fumaric acid; the emulsifier is at least one of alkyl sulfate and alkyl sulfonate. The carboxylic styrene-butadiene latex with low glass transition temperature is obtained by the invention, and the comprehensive properties of softness, moisture absorption, bonding strength and wear resistance are endowed.
Description
Technical Field
The invention relates to the technical field of styrene-butadiene latex, in particular to regenerated carboxylic styrene-butadiene latex for leather and a preparation method thereof.
Background
The artificial leather is made up by using various PVC and PU with different formulas and making them pass through the processes of foaming or film-covering treatment on the basis of woven fabric base or non-woven fabric base, and the styrene-butadiene latex is a stable emulsion made up by using butadiene and styrene through the processes of low-temp. polymerization, and has the important action for adhesion and surface treatment of leather. Can be used for bonding the leather with the base fabric, and can be mixed with small-area broken leather to be reshaped to obtain the whole leather.
Chinese invention with publication number CN104211858B and publication date 2015, 12 and 30 discloses a novel emulsion for children, which is prepared from styrene, butadiene, acrylic acid, seed gum, emulsifier, functional monomer, sodium pyrophosphate, mercaptan, chelating agent ammonium persulfate and other components. The invention also discloses a preparation method of the carboxylic styrene-butadiene latex, wherein an ultrasonic irradiation device is arranged on the side wall of the reaction kettle, the power of the ultrasonic irradiation device is 600-1000W, the ultrasonic frequency can be 60-80 khz, and the power density of the sound wave can be 2-5W/cm2。
In practical use, most of the styrene-butadiene latex is applied to paper, and the requirement on the softness of the coated product is not high. The requirement of leather on softness is high, and after the styrene-butadiene latex and the crushed leather are mixed, the softness of the leather is insufficient after the styrene-butadiene latex is applied to the leather, so that the quality of the leather is directly influenced.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the regenerated carboxylic styrene-butadiene latex for leather with high softness.
The invention also aims to provide a preparation method of the regenerated carboxylic styrene-butadiene latex for leather, which can obtain stable and uniform styrene-butadiene latex.
In order to achieve the first object, the invention provides the following technical scheme:
the technical purpose of the invention is realized by the following technical scheme: the regenerated carboxylic styrene-butadiene latex for leather comprises the following components in parts by weight:
100 parts of main monomer;
80-110 parts of water;
2-4 parts of a functional monomer;
2-3 parts of auxiliary monomer;
0.7-1.2 parts of an initiator;
1-2 parts of a crosslinking agent;
2-3.5 parts of an emulsifier;
3-6 parts of an antioxidant;
the main monomer consists of 50-60% of styrene and the balance of butadiene;
the functional monomer is composed of at least one of itaconic acid, acrylic acid, methacrylic acid and fumaric acid;
the emulsifier is at least one of alkyl sulfate and alkyl sulfonate.
By adopting the technical scheme, the comprehensive proportion of the main monomers is matched with other raw materials, so that the obtained latex has lower Tg temperature, low Tg temperature and low lowest temperature of free movement of macromolecular continuous segments, and the product can more easily embody high elasticity above the temperature; after the low Tg temperature is obtained, the styrene-butadiene latex is adhered between the leather and the cloth layer, so that the influence on the softness of the leather is reduced to the greatest extent, and the excellent softness of the leather is shown after the styrene-butadiene latex is used on the leather, and the excellent softness can be shown at a low temperature. The alkyl sulfate and the alkyl sulfonate belong to nonionic emulsifiers, and can reduce the chemical stability of the latex pad, so that emulsion breaking and leather broken skin mixing forming are easy to realize. Antioxidants can provide weatherability to the product.
More preferably: the functional monomer is prepared from the following components in parts by mass (0.5-1): 1 of acrylic acid and fumaric acid.
By adopting the technical scheme, experiments show that the functional monomer with the composition can obtain better bonding strength.
More preferably: the auxiliary monomer is at least one of acrylonitrile and methacrylonitrile.
By adopting the technical scheme, the acrylonitrile and the methacrylonitrile in the proportion are selected as the auxiliary monomers, so that the adhesive property of the latex can be improved.
More preferably: the auxiliary monomer comprises the following components in parts by mass (0.5-0.65): 1 of acrylonitrile and methacrylonitrile.
By adopting the technical scheme, the acrylonitrile and the methacrylonitrile in the proportion are selected as the auxiliary monomers, so that the adhesive property of the latex can be improved, and the adhesive strength of the latex to leather is improved.
More preferably: the cross-linking agent is N-hydroxymethyl acrylamide.
By adopting the technical scheme, the N-hydroxymethyl acrylamide is a cross-linking monomer with wide application, can be used for adhesives and leather surface treating agents, and has good cross-linking effect.
More preferably: the emulsifier is sodium dodecyl sulfate, and the initiator is ammonium persulfate.
By adopting the technical scheme, the sodium dodecyl sulfate can be used as an emulsifier to provide a bridge for the fusion of a water phase and an oil phase, and the ammonium persulfate acts on a polymerization initiator to be used for the polymerization reaction of the emulsion and the water solution.
In order to achieve the second object, the invention provides the following technical scheme: a preparation method of regenerated carboxylic styrene-butadiene latex for leather comprises the following steps:
s1: uniformly mixing the main monomer and the auxiliary monomer to obtain an oil phase mixture;
s2: uniformly mixing part of water, an emulsifier, a functional monomer, a cross-linking agent and an antioxidant to obtain a water-phase mixture;
s3: mixing and dissolving an initiator and the rest water to obtain a solution A;
s4: taking out part of the water phase mixture, stirring at a stirring speed of 60rpm, heating to 75 ℃, adding part of the solution A, continuously heating to 92 +/-1 ℃, preserving heat, and continuously stirring for 30min to obtain a mixture B;
s5: keeping the stirring speed of 60rpm in S4 and the heat preservation of 92 +/-1 ℃, simultaneously adding the rest water-phase mixture and the solution A into the mixture B at a constant speed, respectively, finishing the addition of the water-phase mixture for 3.5 hours, finishing the addition of the solution A4h, and after finishing the addition of the solution A, stirring and preserving the heat for 2.5 hours to obtain a mixture C;
s6: transferring the mixture C to a degassing kettle for degassing, and adjusting the pH of the mixture C to 7-8 by using a pH regulator;
the S1, S2 and S3 may be performed synchronously;
the water used in the step S2 accounts for 65-70% of the total water amount;
the water phase mixture used in the step S4 accounts for 50-60% of the total amount of the water phase mixture, and the solution A accounts for 40-50% of the total amount of the solution A.
By adopting the technical scheme, the stable, uniform, wear-resistant, soft and high-bonding-strength styrene-butadiene latex is obtained.
More preferably: in step S6, the pH regulator is 35wt% sodium hydroxide solution.
By adopting the technical scheme, the method has the advantages that,
in conclusion, the invention has the following beneficial effects:
1. by adopting the blending of the main monomers and the matching of the main monomers and other raw materials, the styrene-butadiene latex with low glass transition temperature and high softness is obtained, and after the styrene-butadiene latex is used on leather, the excellent softness of the leather is shown.
2. The use of acrylonitrile and methacrylonitrile can improve the adhesive strength of the styrene-butadiene latex.
Detailed Description
Examples 1 to 7: the regenerated carboxylic styrene-butadiene latex for leather comprises the components and the corresponding mass shown in Table 1, and is prepared by the following steps:
s1: weighing and adding the main monomer and the auxiliary monomer into a first stirring kettle, and stirring for 5min at a stirring speed of 120rpm to obtain an oil phase mixture;
s2: weighing 65% of water, an emulsifier, a functional monomer, a cross-linking agent and an antioxidant, putting the water, the emulsifier, the functional monomer, the cross-linking agent and the antioxidant into a second stirring kettle, and stirring for 3min at a stirring speed of 100rpm to obtain a water phase mixture;
s3: weighing and adding the initiator and the rest water into a third stirring kettle, and dissolving to obtain a solution A;
s4: taking out 50% of the water phase mixture, adding into a fourth stirring kettle, heating at a stirring speed of 60rpm, adding 40% of the solution A when the temperature is raised to 75 ℃, continuously heating to 92 +/-1 ℃, keeping the temperature, and continuously stirring for 30min to obtain a mixture B;
s5: keeping the stirring speed of 60rpm and the heat preservation of 92 +/-1 ℃ in a fourth stirring kettle, adding the rest of aqueous phase mixture and the rest of solution A into two metering pumps respectively, simultaneously starting to add into the mixture B at a constant speed, finishing adding the aqueous phase mixture for 3.5 hours, finishing adding the solution A4h, and after finishing adding the solution A, stirring and preserving the heat for 2.5 hours to obtain a mixture C;
s6: transferring the mixture C to a degassing kettle for degassing, and adjusting the pH of the mixture C to 7-8 by using a pH regulator;
s1, S2, and S3 may be performed synchronously;
the pH regulator is 35wt% sodium hydroxide solution.
TABLE 1 examples 1-7 compositions and corresponding masses (kg)
In example 7, the mass part ratio of acrylonitrile to methacrylonitrile was 0.65: 1.
embodiment 8, a method for preparing a recycled carboxylated styrene-butadiene latex for leather, comprising the following steps:
s1: weighing and adding the main monomer and the auxiliary monomer into a first stirring kettle, and stirring for 5min at a stirring speed of 120rpm to obtain an oil phase mixture;
s2: weighing 70% of water, an emulsifier, a functional monomer, a cross-linking agent and an antioxidant, putting the water, the emulsifier, the functional monomer, the cross-linking agent and the antioxidant into a second stirring kettle, and stirring for 3min at a stirring speed of 100rpm to obtain a water phase mixture;
s3: weighing and adding the initiator and the rest water into a third stirring kettle, and dissolving to obtain a solution A;
s4: taking out 60% of the water phase mixture, adding into a fourth stirring kettle, heating at a stirring speed of 60rpm, adding 50% of the solution A when the temperature is raised to 75 ℃, continuously heating to 92 +/-1 ℃, keeping the temperature, and continuously stirring for 30min to obtain a mixture B;
s5: keeping the stirring speed of 60rpm and the heat preservation of 92 +/-1 ℃ in a fourth stirring kettle, adding the rest of aqueous phase mixture and the rest of solution A into two metering pumps respectively, simultaneously starting to add into the mixture B at a constant speed, finishing adding the aqueous phase mixture for 3.5 hours, finishing adding the solution A4h, and after finishing adding the solution A, stirring and preserving the heat for 2.5 hours to obtain a mixture C;
s6: transferring the mixture C to a degassing kettle for degassing, and adjusting the pH of the mixture C to 7-8 by using a pH regulator;
s1, S2, and S3 may be performed synchronously;
the pH regulator is 35wt% sodium hydroxide solution.
Comparative examples 1 to 3: the difference from example 1 is that the components included and the corresponding masses are shown in table 2:
TABLE 2 comparative examples 1-3 components and corresponding masses (kg)
Characterization experiment:
1. solid content, pH, Tg and viscosity determination experiments
Subject: the coatings prepared according to the formulations in examples 1-7 and comparative examples 1-3, for a total of 10 experimental samples.
The experimental method comprises the following steps: solid content, pH, Tg and viscosity measurements were performed on each sample of the stock. The pH was measured with a pH meter. The viscosity was measured using a model NDJ-1 rotational viscometer, #2, test conditions: 60rpm 25 ℃. And (3) Tg measurement: dilatometer method.
Solid content determination: baking flat-bottomed disc (diameter 75mm) in 150 + & lt 2 & gt air blowing box for 15min, cooling to room temperature in drier, weighing and obtaining mass m of flat-bottomed disc0(ii) a Adding 1g of a real sample into the flat-bottomed disc, and ensuring that the sample is uniformly dispersed on the disc surface; placing the flat-bottomed disc filled with the sample into a blast box preheated to 150 +/-2 ℃, keeping for 25min, transferring the flat-bottomed disc into a dryer, cooling to room temperature, and weighing to obtain m1. Solid content%1-m0)/1。
The qualified range value of the solid content is 50 +/-1 percent, the qualified range value of the pH value is 7.0-8.0, and the viscosity is less than or equal to 300 MPa.s.
The experimental results are as follows: the results of the solids content, pH, Tg and viscosity measurements are reported in table 3.
TABLE 3 solid content, pH, Tg and viscosity measurement test results
And (3) data analysis: as can be seen from the data in Table 3, the solids content, pH value and viscosity of the examples are up to standard, the solids content of the comparative example 1 is not up to standard, and the viscosity is lower than that of the examples; meanwhile, the Tg of the examples is about-10 ℃, while the lowest Tg of the comparative example can only reach 7 ℃, and the lower the Tg temperature is, the more the styrene-butadiene latex can show high elasticity state at low temperature, thereby not affecting the softness of leather.
2. Adhesion Strength test
(1) Layer adhesion Strength test
Subject: examples 1-7 and comparative examples 1-3, for a total of 10 experimental groups.
The experimental method comprises the following steps: preparing a leather surface and a cotton textile base fabric, cutting 10 pieces of the leather surface and the cotton textile base fabric into 10cm by 30cm respectively, protruding a force application end with 5cm by 5cm outwards from a wide edge, and enabling each leather surface and the cotton textile base fabric to correspond to one experimental sample. The prepared experimental sample was applied to an area of 10cm x 30cm of a cotton textile substrate, and a portion of 10cm x 30cm of the leather side was adhered to the cotton textile substrate to obtain leather products, which correspond to examples 1 to 7 and comparative examples 1 to 3, respectively. The samples 1 to 7 and the samples 1 to 3 were put into an oven, baked at 60 ℃ for 10min, and then taken out for adhesion test.
Adhesion strength test: punching at the area part center of 5cm x 5cm of leather face and cotton textile base cloth to hang leather goods on the couple through hanging the hole of leather face, fixed a rope in the hole of cotton textile base cloth, the business other end is fixed with 500g weight, before the test, the weight is on the desktop, does not apply force to leather goods. When the test is started, the weight is moved to a position where the lower end face is flush with the lower end face of the leather product, and dropped, and after instantaneous peeling, the peeling distance (cm) between the leather face and the cotton textile base fabric is measured.
The experimental results are as follows: the results of the layer adhesion strength test are reported in table 4.
TABLE 4 record of the results of the layer adhesion Strength test
And (3) data analysis: as is clear from the data in Table 4, the peel distance of the examples was within 1.3cm, showing better adhesive strength, as compared with the peel distance of the comparative examples. The stripping data of the comparative example shows that the ratio of the main monomer, the use ratio and the use ratio of the auxiliary monomer, and the selection and the use ratio of the functional monomer all affect the adhesive strength of the styrene-butadiene latex.
Examples 4-7, which used the preferred ratios of the secondary functional monomers, exhibited better bond strengths than examples 1-3, while examples 6-7, which used the preferred secondary monomers and the preferred functional monomers and their ratios, exhibited greater bond strengths than examples 1-5. Comparative example 3, in which an auxiliary monomer was used, also had better adhesive strength than comparative examples 1-2.
The above-mentioned embodiments are merely illustrative and not restrictive, and those skilled in the art can modify the embodiments without inventive contribution as required after reading this specification, but only fall within the scope of the claims of the present invention.
Claims (8)
1. The regenerated carboxylic styrene-butadiene latex for leather is characterized by comprising the following components in parts by weight:
100 parts of main monomer;
80-110 parts of water;
2-4 parts of a functional monomer;
2-3 parts of auxiliary monomer;
0.7-1.2 parts of an initiator;
1-2 parts of a crosslinking agent;
2-3.5 parts of an emulsifier;
3-6 parts of an antioxidant;
the main monomer consists of 50-60% of styrene and the balance of butadiene;
the functional monomer is composed of at least one of itaconic acid, acrylic acid, methacrylic acid and fumaric acid;
the emulsifier is at least one of alkyl sulfate and alkyl sulfonate.
2. The regenerated carboxylic styrene-butadiene latex for leather according to claim 1, wherein the functional monomer is prepared from the following components in parts by mass (0.5-1): 1 of acrylic acid and fumaric acid.
3. The recycled carboxylated styrene-butadiene latex for leather as claimed in claim 2, wherein said auxiliary monomer is at least one of acrylonitrile and methacrylonitrile.
4. The regenerated carboxylic styrene-butadiene latex for leather according to claim 3, wherein the auxiliary monomer is prepared from (0.5-0.65) by weight: 1 of acrylonitrile and methacrylonitrile.
5. The recycled carboxylated styrene-butadiene latex for leather as claimed in claim 2, wherein said cross-linking agent is N-methylol acrylamide.
6. The recycled carboxylated styrene-butadiene latex for leather as claimed in claim 2, wherein said emulsifier is sodium dodecyl sulfate and said initiator is ammonium persulfate.
7. The method for preparing the regenerated carboxylic styrene-butadiene latex for leather according to claims 1 to 7, which is characterized by comprising the following steps:
s1: uniformly mixing the main monomer and the auxiliary monomer to obtain an oil phase mixture;
s2: uniformly mixing part of water, an emulsifier, a functional monomer, a cross-linking agent and an antioxidant to obtain a water-phase mixture;
s3: mixing and dissolving an initiator and the rest water to obtain a solution A;
s4: taking out part of the water phase mixture, stirring at a stirring speed of 60rpm, heating to 75 ℃, adding part of the solution A, continuously heating to 92 +/-1 ℃, preserving heat, and continuously stirring for 30min to obtain a mixture B;
s5: keeping the stirring speed of 60rpm in S4 and the heat preservation of 92 +/-1 ℃, simultaneously adding the rest water-phase mixture and the solution A into the mixture B at a constant speed, respectively, finishing the addition of the water-phase mixture for 3.5 hours, finishing the addition of the solution A4h, and after finishing the addition of the solution A, stirring and preserving the heat for 2.5 hours to obtain a mixture C;
s6: transferring the mixture C to a degassing kettle for degassing, and adjusting the pH of the mixture C to 7-8 by using a pH regulator;
the S1, S2 and S3 may be performed synchronously;
the water used in the step S2 accounts for 65-70% of the total water amount;
the water phase mixture used in the step S4 accounts for 50-60% of the total amount of the water phase mixture, and the solution A accounts for 40-50% of the total amount of the solution A.
8. The method as claimed in claim 7, wherein in step S6, the pH regulator is 35wt% NaOH solution.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102731724A (en) * | 2012-07-24 | 2012-10-17 | 江苏利田科技股份有限公司 | Washable anti-aging carboxy styrene-butadiene latex for carpet back coating as well as preparation method and application of latex |
| CN103755872A (en) * | 2013-12-23 | 2014-04-30 | 日照广大建筑材料有限公司 | Preparation method of carboxylic butadiene-styrene latex for printed carpet |
| CN107936165A (en) * | 2017-12-12 | 2018-04-20 | 杭州龙驹合成材料有限公司 | A kind of carboxylic styrene butadiene latex and its preparation process |
| CN109354652A (en) * | 2018-10-25 | 2019-02-19 | 杭州龙驹合成材料有限公司 | Carpet carboxylic styrene butadiene latex and preparation method thereof |
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2020
- 2020-01-19 CN CN202010060721.7A patent/CN111154020A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102731724A (en) * | 2012-07-24 | 2012-10-17 | 江苏利田科技股份有限公司 | Washable anti-aging carboxy styrene-butadiene latex for carpet back coating as well as preparation method and application of latex |
| CN103755872A (en) * | 2013-12-23 | 2014-04-30 | 日照广大建筑材料有限公司 | Preparation method of carboxylic butadiene-styrene latex for printed carpet |
| CN107936165A (en) * | 2017-12-12 | 2018-04-20 | 杭州龙驹合成材料有限公司 | A kind of carboxylic styrene butadiene latex and its preparation process |
| CN109354652A (en) * | 2018-10-25 | 2019-02-19 | 杭州龙驹合成材料有限公司 | Carpet carboxylic styrene butadiene latex and preparation method thereof |
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