CN112280130A - Method for preparing latex film product by using polyisoprene latex - Google Patents
Method for preparing latex film product by using polyisoprene latex Download PDFInfo
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- CN112280130A CN112280130A CN202011198577.XA CN202011198577A CN112280130A CN 112280130 A CN112280130 A CN 112280130A CN 202011198577 A CN202011198577 A CN 202011198577A CN 112280130 A CN112280130 A CN 112280130A
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- latex
- aqueous dispersion
- zinc
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- polyisoprene
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- 229920000126 latex Polymers 0.000 title claims abstract description 153
- 239000004816 latex Substances 0.000 title claims abstract description 153
- 229920001195 polyisoprene Polymers 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 43
- RKQOSDAEEGPRER-UHFFFAOYSA-L zinc diethyldithiocarbamate Chemical compound [Zn+2].CCN(CC)C([S-])=S.CCN(CC)C([S-])=S RKQOSDAEEGPRER-UHFFFAOYSA-L 0.000 claims abstract description 38
- BOXSVZNGTQTENJ-UHFFFAOYSA-L zinc dibutyldithiocarbamate Chemical compound [Zn+2].CCCCN(C([S-])=S)CCCC.CCCCN(C([S-])=S)CCCC BOXSVZNGTQTENJ-UHFFFAOYSA-L 0.000 claims abstract description 34
- GIUBHMDTOCBOPA-UHFFFAOYSA-N 3h-1,3-benzothiazole-2-thione;zinc Chemical compound [Zn].C1=CC=C2SC(S)=NC2=C1 GIUBHMDTOCBOPA-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000002360 preparation method Methods 0.000 claims abstract description 19
- 239000002313 adhesive film Substances 0.000 claims abstract description 12
- 239000006185 dispersion Substances 0.000 claims description 55
- 239000003795 chemical substances by application Substances 0.000 claims description 43
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical group [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 29
- 238000004073 vulcanization Methods 0.000 claims description 25
- 230000003712 anti-aging effect Effects 0.000 claims description 19
- 239000000701 coagulant Substances 0.000 claims description 17
- 239000003381 stabilizer Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 15
- 239000011593 sulfur Substances 0.000 claims description 15
- 239000011787 zinc oxide Substances 0.000 claims description 14
- IWDCLRJOBJJRNH-UHFFFAOYSA-N p-cresol Chemical compound CC1=CC=C(O)C=C1 IWDCLRJOBJJRNH-UHFFFAOYSA-N 0.000 claims description 12
- 229910052717 sulfur Inorganic materials 0.000 claims description 12
- 239000012190 activator Substances 0.000 claims description 11
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical group [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 8
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 8
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 claims description 7
- 238000007598 dipping method Methods 0.000 claims description 7
- 229920001971 elastomer Polymers 0.000 claims description 7
- 239000003292 glue Substances 0.000 claims description 7
- 239000005060 rubber Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 159000000007 calcium salts Chemical class 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000012936 vulcanization activator Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- PGNWIWKMXVDXHP-UHFFFAOYSA-L zinc;1,3-benzothiazole-2-thiolate Chemical compound [Zn+2].C1=CC=C2SC([S-])=NC2=C1.C1=CC=C2SC([S-])=NC2=C1 PGNWIWKMXVDXHP-UHFFFAOYSA-L 0.000 claims description 5
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 229910001424 calcium ion Inorganic materials 0.000 claims description 4
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical group [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 4
- 235000013539 calcium stearate Nutrition 0.000 claims description 4
- 239000008116 calcium stearate Substances 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 238000002386 leaching Methods 0.000 claims description 4
- 239000003963 antioxidant agent Substances 0.000 claims description 3
- 230000003078 antioxidant effect Effects 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical group O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- SZRLKIKBPASKQH-UHFFFAOYSA-M dibutyldithiocarbamate Chemical compound CCCCN(C([S-])=S)CCCC SZRLKIKBPASKQH-UHFFFAOYSA-M 0.000 claims 1
- 229940116901 diethyldithiocarbamate Drugs 0.000 claims 1
- LMBWSYZSUOEYSN-UHFFFAOYSA-N diethyldithiocarbamic acid Chemical compound CCN(CC)C(S)=S LMBWSYZSUOEYSN-UHFFFAOYSA-N 0.000 claims 1
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 abstract description 14
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 8
- 229910021529 ammonia Inorganic materials 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 abstract 1
- 238000007711 solidification Methods 0.000 abstract 1
- 230000008023 solidification Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 15
- 239000000126 substance Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 102000004169 proteins and genes Human genes 0.000 description 8
- 108090000623 proteins and genes Proteins 0.000 description 8
- OWRCNXZUPFZXOS-UHFFFAOYSA-N 1,3-diphenylguanidine Chemical compound C=1C=CC=CC=1NC(=N)NC1=CC=CC=C1 OWRCNXZUPFZXOS-UHFFFAOYSA-N 0.000 description 6
- 239000000853 adhesive Substances 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 6
- 229910052761 rare earth metal Inorganic materials 0.000 description 5
- 150000002910 rare earth metals Chemical class 0.000 description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- 229920001194 natural rubber Polymers 0.000 description 4
- 229920003051 synthetic elastomer Polymers 0.000 description 4
- 244000043261 Hevea brasiliensis Species 0.000 description 3
- TXKMVPPZCYKFAC-UHFFFAOYSA-N disulfur monoxide Inorganic materials O=S=S TXKMVPPZCYKFAC-UHFFFAOYSA-N 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 229920003052 natural elastomer Polymers 0.000 description 3
- 239000005061 synthetic rubber Substances 0.000 description 3
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 description 2
- UXMWYAHQOASHPK-UHFFFAOYSA-N 4-sulfanyl-3h-1,3-benzothiazole-2-thione;zinc Chemical compound [Zn].SC1=CC=CC2=C1NC(=S)S2 UXMWYAHQOASHPK-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 102000011632 Caseins Human genes 0.000 description 2
- 108010076119 Caseins Proteins 0.000 description 2
- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical compound NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 208000003455 anaphylaxis Diseases 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229940080237 sodium caseinate Drugs 0.000 description 2
- KUAZQDVKQLNFPE-UHFFFAOYSA-N thiram Chemical compound CN(C)C(=S)SSC(=S)N(C)C KUAZQDVKQLNFPE-UHFFFAOYSA-N 0.000 description 2
- 229960002447 thiram Drugs 0.000 description 2
- 206010002198 Anaphylactic reaction Diseases 0.000 description 1
- 206010002199 Anaphylactic shock Diseases 0.000 description 1
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 1
- 208000005623 Carcinogenesis Diseases 0.000 description 1
- 201000004624 Dermatitis Diseases 0.000 description 1
- 206010016946 Food allergy Diseases 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- FCSHMCFRCYZTRQ-UHFFFAOYSA-N N,N'-diphenylthiourea Chemical compound C=1C=CC=CC=1NC(=S)NC1=CC=CC=C1 FCSHMCFRCYZTRQ-UHFFFAOYSA-N 0.000 description 1
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 208000026935 allergic disease Diseases 0.000 description 1
- 230000007815 allergy Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000036952 cancer formation Effects 0.000 description 1
- 231100000504 carcinogenesis Toxicity 0.000 description 1
- 229920003211 cis-1,4-polyisoprene Polymers 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229920006173 natural rubber latex Polymers 0.000 description 1
- 210000002445 nipple Anatomy 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- XKLJHFLUAHKGGU-UHFFFAOYSA-N nitrous amide Chemical compound ON=N XKLJHFLUAHKGGU-UHFFFAOYSA-N 0.000 description 1
- 125000000552 p-cresyl group Chemical group [H]C1=C([H])C(=C([H])C([H])=C1O*)C([H])([H])[H] 0.000 description 1
- 229920001084 poly(chloroprene) Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/02—Direct processing of dispersions, e.g. latex, to articles
-
- 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
- C08J2309/00—Characterised by the use of homopolymers or copolymers of conjugated diene hydrocarbons
- C08J2309/10—Latex
-
- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/06—Sulfur
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/39—Thiocarbamic acids; Derivatives thereof, e.g. dithiocarbamates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/45—Heterocyclic compounds having sulfur in the ring
- C08K5/46—Heterocyclic compounds having sulfur in the ring with oxygen or nitrogen in the ring
- C08K5/47—Thiazoles
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- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The invention belongs to the technical field of latex film products, and particularly relates to a method for preparing a latex film product by using polyisoprene latex. The method comprises the following steps: preparing the complex latex, preparing the solidification liquid, preparing the adhesive film and preparing the latex film product. The accelerators used for preparing the compounded latex are zinc diethyldithiocarbamate, zinc dibutyldithiocarbamate and zinc 2-mercaptobenzothiazole. The latex film product obtained by the invention has high elongation at break, high tensile strength and better transparency than natural latex, and the preparation process does not have pungent ammonia smell of the natural latex, thereby realizing green production of the latex product.
Description
Technical Field
The invention belongs to the technical field of latex film products, and particularly relates to a method for preparing a latex film product by using polyisoprene latex.
Background
Natural latex has always dominated the latex article field. Due to the unique and superior properties of natural rubber latex in the production of surgical gloves, balloons, condoms and the like, other materials are difficult to replace. The natural latex mainly comprises cis-1, 4-polyisoprene, water and non-gum substances, wherein the non-gum substances mainly comprise protein, lipoid, acetone soluble substances, water soluble substances, inorganic salt and the like. The non-glue material mainly contains protein, the fresh natural latex contains 1-2% of protein, the concentrated latex contains 1.5-3.5% of protein, and after the product is processed by dipping, leaching, vulcanizing, washing and other processing procedures, a considerable amount of soluble protein still remains in the product. When a user touches latex containing a certain protein, contact allergy such as dermatitis is often caused, and even severe cases may cause anaphylactic shock. In addition, the water absorption of protein causes the hygroscopicity, conductivity and heat generation of natural latex products, which are disadvantageous for the production of insulating products, and the product is liable to get moldy when the protein content is too high. Therefore, it is urgent to find substitutes for natural latex, and various synthetic materials have been used as substitutes for natural latex. Synthetic latexes such as nitrile latex, neoprene latex, and the like have been used in the production of surgical and examination gloves. However, none of these materials have the high elasticity and resilience of natural rubber.
In the synthetic rubber, the performance of polyisoprene rubber is the closest to that of natural rubber, and the system is pure and does not contain non-rubber components, thereby not causing protein anaphylactic reaction of human bodies. Therefore, the polyisoprene rubber is taken as a raw material, the polyisoprene latex prepared by a solution emulsification method contains few surfactants and anti-aging agents and also does not contain other non-rubber components, the problems of protein allergy, nitrosamine carcinogenesis and the like existing in natural rubber can be better solved, and the performance of the polyisoprene latex is similar to that of the natural latex, so the polyisoprene rubber can partially or completely replace the natural latex to be used for manufacturing dipping products, rubber threads, adhesives, sponge products and the like.
The production of latex products by dipping plays an important role in the latex industry, being the method which is the earliest, the most common and the most productive. The produced varieties comprise various gloves, balloons, condoms, nipples and the like. The sizing material used in the dipping application can be used either as a compounded latex or as a pre-vulcanized latex, but most importantly, the latex must have good film forming properties. Generally, vulcanized latex is used for thin products, and compounded latex is used for thick products. The ingredient dispersion and emulsion particles added into the latex are ground as finely as possible, so that the ingredients are uniformly dispersed in the latex and are not easy to aggregate and settle. The adhesive material of the thin product requires high dry adhesive content, but low viscosity, the adhesive material of the thick product not only requires high dry adhesive content, but also requires high viscosity within the allowable range of the process, and the adhesive material can not only prevent the precipitation of the compounding ingredients, but also obtain thicker adhesive films.
In dipping products of latex, the main research on synthetic and natural polyisoprene latex has focused on the vulcanization system and the prevulcanisation process. As early as 1914, Hidesravitz invented and patented a latex vulcanization process.
In the preparation of film articles using polyisoprene latex, problems have been found in that the tensile strength of the resulting articles is not high and the conditions for pre-vulcanization are relatively severe.
U.S. Pat. No. 4,6828387 discloses a polyisoprene latex product and a process for its preparation. The vulcanization system is that 0.5 part of Zinc Diethyldithiocarbamate (ZDEC), 0.5 part of zinc dimercaptobenzothiazole (ZMBT), 1.00 part of diphenyl guanidine (DPG), 0.5 part of zinc oxide, 1.25 parts of sulfur, 0.75 part of sodium caseinate and 2.00 parts of anti-aging agent Wingstay are added into each hundred parts of the systemTMAnd L. In the embodiment, polyisoprene latex with solid content of 60% is firstly mixed with sodium caseinate serving as a stabilizer uniformly at room temperature of 20-25 ℃. Then adding an anti-aging agent windstayTML, stirringStirring and mixing for 15 min. While stirring was maintained, a mixture of zinc oxide, sulfur and the three accelerators was added and diluted with distilled water to a solids content of about 40% and the pH was adjusted to about 10 with ammonia. Stirring was then continued for 24h below 25 ℃. The complex latex has high stability, can be stored for 8 days at 15-20 ℃, and the prepared glove product has the tensile strength of 3000psi (20.6MPa) and the elongation at break of 750 percent (test standard: ASTM D412). However, the accelerator system used by the method contains guanidine accelerators, and the accelerator can change color and is polluting after being irradiated by light and is not suitable for white and light-colored products and products contacting with food.
US patent 6618861 discloses a process for making medical gloves with watch viewing function from latex. The vulcanization system of example 2 was prepared by adding 0.2 parts of Zinc Diethyldithiocarbamate (ZDEC), 0.2 parts of zinc dimercaptobenzothiazole (ZMBT), 0.2 parts of Zinc Dibutyldithiocarbamate (ZDBC), 2.0 parts of tetramethylthiuram disulfide (TMTD), 0.2 parts of 1, 3-diphenyl-2-thiourea (CA), 0.5 parts of zinc oxide, 0.3 parts of sulfur, 0.5 parts of titanium dioxide and 0.2 parts of antioxidant 264 per hundred parts of the system. The tensile strength of the product prepared by the vulcanization system is 13.22MPa, the elongation at break is 1028 percent, and the 300 percent stress at definite elongation is 1.03. The patent aims to invent a glove with watch viewing function, 5 accelerators are selected, a vulcanization system is complex, the tensile strength of a product is low, and the patent does not relate to production process parameters at all.
Chinese patent CN101029163A discloses a method for making gloves and related products from polyisoprene water-based latex. The vulcanization system of example 3 was such that 2.0 parts of sulfur, 1.0 part of zinc oxide, and 1 part of accelerator Zinc Dibutyldithiocarbamate (ZDBC) were added per 100 parts of polyisoprene emulsion. The glove prepared by the vulcanization system has the tensile strength of 14MPa, the elongation at break of 600 percent, good hand feeling and strong rebound resilience. However, the polyisoprene latex glove to which this patent relates does not meet the requirements of ASTM D3577-09(2015) standards for synthetic rubber surgical gloves in terms of tensile strength and elongation at break.
Disclosure of Invention
The invention aims to provide a method for preparing a latex film product by using polyisoprene latex, the obtained latex film product has high elongation at break, high tensile strength and better transparency than natural latex, and the preparation process has no pungent ammonia smell of the natural latex, so that the green production of the latex product can be realized.
The method for preparing the latex film product by using the polyisoprene latex comprises the steps of preparing a compound latex, preparing a coagulant, preparing a glue film and preparing the latex film product; wherein the step of preparing the complex latex comprises: the dry-state proportioning dosage of the stabilizer, the pH regulator, the vulcanizing agent, the vulcanization activator, the accelerator and the anti-aging agent is as follows by 100 parts of polyisoprene latex:
0.2-1.5 parts of a stabilizer;
0.1-0.3 part of pH regulator;
2.0-2.5 parts of a vulcanizing agent;
1.5-2.0 parts of a vulcanization activator;
1.2-1.5 parts of an accelerator;
1.0-2.0 parts of an anti-aging agent.
Wherein:
the accelerator is Zinc Diethyldithiocarbamate (ZDEC), Zinc Dibutyldithiocarbamate (ZDBC) and zinc 2-mercaptobenzothiazole (ZMBT); the dry ratio of Zinc Diethyldithiocarbamate (ZDEC) to Zinc Dibutyldithiocarbamate (ZDBC) is 1-2:1, preferably 1:1, 2:1 and 3: 2; the dry-state proportioning quantity part ratio of the Zinc Diethyldithiocarbamate (ZDEC) and the zinc 2-mercaptobenzothiazole (ZMBT) is 2: 1.
The stabilizer is sodium dodecyl benzene sulfonate; the pH regulator is potassium hydroxide; the vulcanizing agent is sulfur; the vulcanizing activator is zinc oxide; the anti-aging agent is p-cresol and dicyclopentadiene butylated product 616 (anti-aging agent 616).
The method for preparing the latex film product by using the polyisoprene latex specifically comprises the following steps:
(1) preparation of the Complex latex
Respectively preparing a vulcanizing agent, a vulcanizing activator, a promoter and an anti-aging agent into a vulcanizing agent aqueous dispersion, a vulcanizing activator aqueous dispersion, a promoter aqueous dispersion and an anti-aging agent aqueous dispersion; respectively preparing a pH regulator solution and a stabilizer solution from the pH regulator and the stabilizer;
adding a pH regulator solution and a stabilizer solution into polyisoprene latex, sequentially adding a vulcanizing agent aqueous dispersion, a vulcanizing activator aqueous dispersion, an accelerator aqueous dispersion and an anti-aging agent aqueous dispersion, uniformly stirring, and adding distilled water to adjust the solid content to obtain a complex latex;
(2) preparation of the coagulant
Adding a divalent calcium salt and a release agent into water, mixing and heating to prepare a coagulant;
(3) preparation of the adhesive film
Heating the product mould, putting the product mould into the coagulant obtained in the step (2), soaking, drying and cooling; dipping the cooled product mold in the matched latex in the step (1) to obtain a glue film;
(4) preparation of latex film articles
And (4) leaching the adhesive film obtained in the step (3), vulcanizing, coating a release agent on the surface of the adhesive film, and finally demolding to obtain the latex film product.
Wherein:
in the step (1), the polyisoprene latex is prepared by using rare-earth polyisoprene latex as a raw material through 4 working procedures of dissolving, emulsifying, desolventizing and concentrating.
In the step (1), the vulcanizing agent, the vulcanizing activator, the accelerator and the anti-aging agent are firstly ground by a ball mill, the particle size of the vulcanizing agent, the vulcanizing activator, the accelerator and the anti-aging agent is consistent with that of the used polyisoprene latex, then the polyisoprene latex is prepared into water dispersoid, added into the polyisoprene latex, and stirred at low speed for 24 hours at room temperature for mixing to obtain the complex latex. The compounded latex needs to be placed and matured for 1-3 days, and the time for placing and maturing can be controlled by measuring the chloroform value of the compounded latex in the process.
In the step (1), the aqueous accelerator dispersion is an aqueous Zinc Diethyldithiocarbamate (ZDEC) dispersion, an aqueous Zinc Dibutyldithiocarbamate (ZDBC) dispersion and an aqueous 2-mercaptobenzothiazole zinc salt (ZMBT) dispersion; wherein the mass percentage concentration of the Zinc Diethyldithiocarbamate (ZDEC) aqueous dispersion, the Zinc Dibutyldithiocarbamate (ZDBC) aqueous dispersion and the zinc 2-mercaptobenzothiazole (ZMBT) aqueous dispersion is 30-50%, preferably 50%; all are environment-friendly vulcanization accelerators, and can obviously improve the tensile strength and the elongation at break of the latex film product.
In the step (1), the mass percentage concentration of the stabilizer solution is 25%; the mass percentage concentration of the pH regulator solution is 10-15%, preferably 10%; the mass percentage concentration of the vulcanizing agent water dispersion is 50-60%, preferably 60%; the mass percentage concentration of the vulcanization activator water dispersion is 30-50%, preferably 50%; the mass percentage concentration of the antioxidant aqueous dispersion is 30-50%, preferably 50%.
In the step (1), the solid content of the complex latex is 35-45%; the pH value is 10.5-11.5 to ensure the stability of the compounded latex.
In the step (2), the mass percent of the divalent calcium salt in the coagulant is 10-20%, and the mass percent of the release agent is 0.5-1.5%; the divalent calcium salt is hydrochloride or nitrate of divalent calcium ions, and the release agent is calcium stearate aqueous dispersion.
In the step (3), the product mold is heated to 100-120 ℃, is placed in the coagulant in the step (2) to be soaked for 10-30 s, is dried at 100-120 ℃, and is cooled to 40-60 ℃; and (3) placing the cooled product mold into the matched latex in the step (1) to dip for 10-30 s, and forming a glue film on the product mold.
In the step (4), the vulcanization temperature is 110-130 ℃, the vulcanization time is 15-35 minutes, and the physical properties of the adhesive film can be reduced when the vulcanization temperature is too high, the vulcanization time is not enough or too long.
In the step (4), the separant is talcum powder.
The invention has the following beneficial effects:
the Zinc Diethyldithiocarbamate (ZDEC) is an overspeed vulcanization accelerator, has small influence on the stability of latex, is free from pollution, discoloration, odor and toxicity, and can improve the vulcanization speed; zinc Dibutyldithiocarbamate (ZDBC) is also an overspeed vulcanization accelerator, is similar to accelerator ZDEC, but has higher activity and is easy to disperse in latex, and can improve the aging resistance of latex products; the use of Zinc Diethyldithiocarbamate (ZDEC), Zinc Dibutyldithiocarbamate (ZDBC), and zinc 2-mercaptobenzothiazole (ZMBT) together can improve the activity of zinc 2-mercaptobenzothiazole (ZMBT), and is a good activator for zinc 2-mercaptobenzothiazole (ZMBT). The 2-mercaptobenzothiazole zinc salt (ZMBT) has good dispersibility and has the function of adjusting the viscosity of a system in a latex system. The rare earth polyisoprene latex used in the invention has a regular microstructure, the cis-1, 4-structure content of 97 percent, higher relative molecular mass and better physical property. Under the interaction of the 3 accelerators and the sodium dodecyl benzene sulfonate stabilizer, the stability of the complex latex prepared from the rare-earth polyisoprene latex is better, and the elongation at break and the tensile strength of the latex film product are improved.
According to the invention, the product with the film thickness of 0.1-1.0 mm can be prepared according to the requirement, the tensile strength of the latex film product is more than 20.70MPa, the elongation at break is more than 900%, and the requirements of ASTM D3577-09(2015) standards on synthetic rubber surgical gloves are completely met: the tensile strength is more than or equal to 17MPa, and the elongation at break is more than or equal to 650 percent.
The latex film product obtained by the invention has high elongation at break, high tensile strength and better transparency than natural latex, and the preparation process does not have pungent ammonia smell of the natural latex, thereby realizing green production of the latex product.
Detailed Description
The present invention is further described below with reference to examples.
Examples 1 to 4
The method for preparing the latex film product by using the polyisoprene latex comprises the following steps:
(1) preparation of the Complex latex
Preparing sulfur, zinc oxide, Zinc Diethyldithiocarbamate (ZDEC), Zinc Dibutyldithiocarbamate (ZDBC), zinc 2-mercaptobenzothiazole (ZMBT), and p-cresol and dicyclopentadiene butylated product 616 into an aqueous sulfur dispersion, an aqueous zinc oxide dispersion, an aqueous Zinc Diethyldithiocarbamate (ZDEC), an aqueous Zinc Dibutyldithiocarbamate (ZDBC), an aqueous 2-mercaptobenzothiazole (ZMBT) dispersion, and an aqueous p-cresol and dicyclopentadiene butylated product 616, respectively; respectively preparing potassium hydroxide solution and sodium dodecyl benzene sulfonate solution from potassium hydroxide and sodium dodecyl benzene sulfonate;
wherein the mass percent concentration of the sulfur aqueous dispersion is 60 percent, the mass percent concentration of the zinc oxide aqueous dispersion is 50 percent, the mass percent concentration of the p-cresol and dicyclopentadiene butylated product (anti-aging agent 616) aqueous dispersion is 50 percent, the mass percent concentration of the Zinc Diethyldithiocarbamate (ZDEC) aqueous dispersion, the mass percent concentration of the Zinc Dibutyldithiocarbamate (ZDBC) aqueous dispersion and the mass percent concentration of the 2-mercaptobenzothiazole zinc salt (ZMBT) aqueous dispersion are 50 percent, the mass percent concentration of the potassium hydroxide solution is 10 percent, and the mass percent concentration of the sodium dodecyl benzene sulfonate solution is 25 percent.
Filtering rare earth polyisoprene latex, adding a potassium hydroxide solution and a sodium dodecyl benzene sulfonate solution into the rare earth polyisoprene latex under the stirring state, and then sequentially adding a sulfur aqueous dispersion, a zinc oxide aqueous dispersion, a Zinc Diethyldithiocarbamate (ZDEC) aqueous dispersion, a Zinc Dibutyldithiocarbamate (ZDBC) aqueous dispersion, a 2-mercaptobenzothiazole zinc salt (ZMBT) aqueous dispersion and a p-cresol and dicyclopentadiene butylated product (antioxidant 616) aqueous dispersion; and adding distilled water to adjust the total solid content to be 35-45% and the pH value to be 10.5-11.5, and stirring at the rotating speed of 60rpm for 24 hours at room temperature to mix to obtain the complex latex. The compounded latex needs to be placed and matured for 1-3 days, and the time for placing and maturing can be controlled by measuring the chloroform value of the compounded latex in the process. Wherein, the dry state proportioning dosage of each substance is shown in table 1.
(2) Preparation of the coagulant
Adding hydrochloride of divalent calcium ions and the calcium stearate aqueous dispersion into water, mixing, heating in a water bath at 55-60 ℃ and stirring for 24-30 hours to obtain a coagulant; wherein the mass percent of the hydrochloride of divalent calcium ions in the coagulant is 10-20%, and the mass percent of the calcium stearate aqueous dispersion in the coagulant is 0.5-1.5%.
(3) Preparation of the adhesive film
Heating a product mold to 100-120 ℃, soaking the product mold in the coagulant obtained in the step (2) for 10-30 s, drying the product mold at 100-120 ℃, and cooling the product mold to 40-60 ℃; and (3) placing the cooled product mold into the matched latex in the step (1) to dip for 10-30 s, and forming a glue film on the product mold.
(4) Preparation of latex film articles
And (4) leaching the adhesive film obtained in the step (3), vulcanizing at 110-130 ℃ for 15-35 minutes, coating talcum powder on the surface of the adhesive film, and finally demolding to obtain the latex film product. The resulting latex film articles were tested for tensile strength and elongation at break, and the data are shown in Table 1.
TABLE 1 Table of the amounts of the respective substances in the compounded latex of examples 1 to 4 and the performance data of the latex film products
Comparative example 1
The materials and amounts of the formulated latex are shown in Table 2, and latex film was prepared according to the method of example 1.
TABLE 2 data Table of substances and amounts in comparative example 1 compounded latex
| Name of each substance | Dry mix ratio (parts by mass) |
| Polyisoprene latex | 100 |
| Sulfur | 2.0 |
| Zinc oxide | 0.5 |
| Zinc diethyl dithiocarbamate (ZDEC) | 0.5 |
| Zinc dibutyl dithiocarbamate (ZDBC) | 0.5 |
| Diphenylguanidine (DPG) | 1.0 |
| Sodium dodecyl benzene sulfonate | 0.4 |
| Butylated products 616 of para-cresol and dicyclopentadiene | 1.5 |
| Potassium hydroxide | 0.1 |
The resulting latex film article was tested to have a tensile strength of 14.7MPa and elongation at break of 930%. The formula is a formula of the latex compounded in the US patent US6828387, and the tensile strength of a latex film product prepared by the formula can not meet the standard requirement of ASTM D3577-09 (2015). The accelerator Diphenylguanidine (DPG) used is discolored by light irradiation, is polluting and is not suitable for white and light-colored products and products in contact with food.
Comparative example 2
The accelerators were Zinc Diethyldithiocarbamate (ZDEC) and Zinc Dibutyldithiocarbamate (ZDBC), the rest of the procedure being as in example 1. The resulting latex film articles were tested for tensile strength and elongation at break, and the data is shown in Table 3.
Comparative example 3
The accelerators were Zinc Dibutyldithiocarbamate (ZDBC) and zinc 2-mercaptobenzothiazole (ZMBT), the procedure being as in example 1. The resulting latex film articles were tested for tensile strength and elongation at break, and the data is shown in Table 3.
Comparative example 4
The accelerators were Zinc Diethyldithiocarbamate (ZDEC) and zinc 2-mercaptobenzothiazole (ZMBT), the procedure being as in example 1. The resulting latex film articles were tested for tensile strength and elongation at break, and the data is shown in Table 3.
TABLE 3 Table of Performance data for comparative examples 2-4 latex film articles
It can be seen from the data in table 3 that the elongation at break of the latex film product obtained with the two accelerators meets the requirements of ASTM D3577-09(2015) standard, but the tensile strength is lower than that of example 1.
Comparative examples 5 to 11
The same procedure as in example 1 was repeated except that the amounts of sulfur, zinc oxide, or both of sulfur and zinc oxide used in example 1 were changed. The resulting latex film articles were tested for tensile strength and elongation at break, and the data is shown in Table 4.
TABLE 4 data table of the dosage of each substance in comparative examples 5-11 and the performance of latex film product
As can be seen from the data in Table 4, the amounts of sulfur and zinc oxide in comparative examples 5-10 are lower than those in example 1, and the elongation at break of the obtained latex film product meets the requirements of ASTM D3577-09(2015) standard, is lower than or higher than that of example 1, but the tensile strength is lower than that of example 1 and does not meet the requirements of ASTM D3577-09(2015) standard; the amount of sulfur and zinc oxide used in comparative example 11 was higher than that used in example 1, and although the tensile strength was high, the elongation at break was lower than that of example 1.
Comparative example 12
The vulcanization temperature in example 1 was changed to 100 ℃ and the procedure was the same as in example 1. The resulting latex film articles were tested for tensile strength and elongation at break, and the data is shown in Table 5.
Comparative example 13
The vulcanization temperature in example 1 was changed to 140 ℃ and the procedure was the same as in example 1. The resulting latex film articles were tested for tensile strength and elongation at break, and the data is shown in Table 5.
Comparative example 14
The vulcanization time in example 1 was changed to 10 minutes, and the procedure was the same as in example 1. The resulting latex film articles were tested for tensile strength and elongation at break, and the data is shown in Table 5.
Comparative example 15
The vulcanization time in example 1 was changed to 40 minutes, and the procedure was the same as in example 1. The resulting latex film articles were tested for tensile strength and elongation at break, and the data is shown in Table 5.
TABLE 5 table of performance data for comparative examples 12-15 latex film articles
As can be seen from the data in Table 5, the tensile strength and elongation at break of the latex film article are reduced when the vulcanization temperature is too high or too low and the vulcanization time is insufficient or too long.
Claims (10)
1. A method for preparing a latex film product by using polyisoprene latex comprises the steps of preparing a compound latex, preparing a coagulant, preparing a rubber film and preparing a latex film product; the method is characterized in that the preparation of the complex latex comprises the following steps: the dry-state proportioning dosage of the stabilizer, the pH regulator, the vulcanizing agent, the vulcanization activator, the accelerator and the anti-aging agent is as follows by 100 parts of polyisoprene latex:
0.2-1.5 parts of a stabilizer;
0.1-0.3 part of pH regulator;
2.0-2.5 parts of a vulcanizing agent;
1.5-2.0 parts of a vulcanization activator;
1.2-1.5 parts of an accelerator;
1.0-2.0 parts of an anti-aging agent.
2. The method of claim 1, wherein the polyisoprene latex is prepared by the method comprising: the accelerator is zinc diethyl dithiocarbamate, zinc dibutyl dithiocarbamate and zinc 2-mercaptobenzothiazole; wherein the dry ratio of zinc diethyldithiocarbamate to zinc dibutyldithiocarbamate is 1-2:1, and the dry ratio of zinc diethyldithiocarbamate to zinc 2-mercaptobenzothiazole is 2: 1.
3. The method of claim 1, wherein the polyisoprene latex is prepared by the method comprising: the stabilizer is sodium dodecyl benzene sulfonate; the pH regulator is potassium hydroxide; the vulcanizing agent is sulfur; the vulcanizing activator is zinc oxide; the anti-aging agent is a butylated product of p-cresol and dicyclopentadiene.
4. A process for the preparation of a latex film article from polyisoprene latex as claimed in any one of claims 1 to 3 which comprises the steps of:
(1) preparation of the Complex latex
Respectively preparing a vulcanizing agent, a vulcanizing activator, a promoter and an anti-aging agent into a vulcanizing agent aqueous dispersion, a vulcanizing activator aqueous dispersion, a promoter aqueous dispersion and an anti-aging agent aqueous dispersion; respectively preparing a pH regulator solution and a stabilizer solution from the pH regulator and the stabilizer;
adding a pH regulator solution and a stabilizer solution into polyisoprene latex, sequentially adding a vulcanizing agent aqueous dispersion, a vulcanizing activator aqueous dispersion, an accelerator aqueous dispersion and an anti-aging agent aqueous dispersion, uniformly stirring, and adding distilled water to adjust the solid content to obtain a complex latex;
(2) preparation of the coagulant
Adding a divalent calcium salt and a release agent into water, mixing and heating to prepare a coagulant;
(3) preparation of the adhesive film
Heating the product mould, putting the product mould into the coagulant obtained in the step (2), soaking, drying and cooling; dipping the cooled product mold in the matched latex in the step (1) to obtain a glue film;
(4) preparation of latex film articles
And (4) leaching the adhesive film obtained in the step (3), vulcanizing, coating a release agent on the surface of the adhesive film, and finally demolding to obtain the latex film product.
5. The method of claim 4, wherein the polyisoprene latex is prepared from a latex film of the polyisoprene latex: in the step (1), the accelerator aqueous dispersion is diethyl dithiocarbamate aqueous dispersion, dibutyl dithiocarbamate aqueous dispersion and 2-mercaptobenzothiazole zinc salt aqueous dispersion; wherein the mass percentage concentration of the zinc diethyldithiocarbamate aqueous dispersion, the zinc dibutyldithiocarbamate aqueous dispersion and the zinc 2-mercaptobenzothiazole aqueous dispersion is 30-50%.
6. The method of claim 4, wherein the polyisoprene latex is prepared from a latex film of the polyisoprene latex: in the step (1), the mass percentage concentration of the stabilizer solution is 25%; the mass percentage concentration of the pH regulator solution is 10-15%; the mass percentage concentration of the vulcanizing agent water dispersion is 50-60%; the mass percentage concentration of the vulcanization activator aqueous dispersion is 30-50%; the mass percentage concentration of the antioxidant aqueous dispersion is 30-50%.
7. The method of claim 4, wherein the polyisoprene latex is prepared from a latex film of the polyisoprene latex: in the step (1), the solid content of the complex latex is 35-45%; the pH value is 10.5-11.5.
8. The method of claim 4, wherein the polyisoprene latex is prepared from a latex film of the polyisoprene latex: in the step (2), the mass percent of the divalent calcium salt in the coagulant is 10-20%, and the mass percent of the release agent is 0.5-1.5%; the divalent calcium salt is hydrochloride or nitrate of divalent calcium ions, and the release agent is calcium stearate aqueous dispersion.
9. The method of claim 4, wherein the polyisoprene latex is prepared from a latex film of the polyisoprene latex: in the step (3), the product mold is heated to 100-120 ℃, is placed in the coagulant in the step (2) to be soaked for 10-30 s, is dried at 100-120 ℃, and is cooled to 40-60 ℃; and (3) placing the cooled product mold into the matched latex in the step (1) to dip for 10-30 s to obtain the glue film.
10. The method of claim 4, wherein the polyisoprene latex is prepared from a latex film of the polyisoprene latex: in the step (4), the vulcanization temperature is 110-130 ℃, and the vulcanization time is 15-35 minutes; the separant is talcum powder.
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