CN104004243B - Hot sulfurization neoprene cement and preparation method thereof - Google Patents

Hot sulfurization neoprene cement and preparation method thereof Download PDF

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CN104004243B
CN104004243B CN201410267613.1A CN201410267613A CN104004243B CN 104004243 B CN104004243 B CN 104004243B CN 201410267613 A CN201410267613 A CN 201410267613A CN 104004243 B CN104004243 B CN 104004243B
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neoprene
mixed solvent
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tackifier
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CN104004243A (en
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江卫东
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Jihua 3539 Shoe Making Co Ltd
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Jihua 3539 Shoe Making Co Ltd
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Abstract

Hot sulfurization neoprene cement of the present invention and preparation method thereof, rubber cement raw material comprises neoprene latex, domestic No. 1 smoked sheet, promotor, indirect process zinc oxide, light magnesium oxide, anti-aging agent, (scorch retarder), white carbon black, tackifier, mixed solvent by weight; Traditional formula is improved; to reduce its toxic, the health of protection operator, can improve again technological operation performance in process for processing simultaneously; simplify preparation technology and operation steps; improve processing and fabricating efficiency, sticking power between sizing material and fabric is improved to finished product, meet slurry, non-discoloring performance thoroughly simultaneously; and then improve the over-all properties of rubber cement; improve product qualified rate, reach energy-saving and cost-reducing object, save Financial cost.

Description

Hot sulfurization neoprene cement and preparation method thereof
Technical field
The present invention relates to a kind of rubber cement, particularly a kind of for making the shaping footwear of laminating method production hot sulfurization neoprene cement used and preparation method thereof.
Background technology
Neoprene cement is widely used among shoemaking production, there is the problem of following several respects for a long time: one, most of neoprene cement uses containing triphen (benzene always, toluene, dimethylbenzene) organic solvent of class, toxicity is very large, very large to the operator's harm in making and use procedure, though through taking various safeguard procedures, still very important to the harm of Long Term Contact person; Two, most of neoprene cement is all only applicable to cold bonding pressing and forming, the kind that can be used for hot sulfurization shaping is little, but for use neoprene latex, the non-polar rubbers such as butadiene-acrylonitrile rubber make the glue stuff compounding of material of main part or moulded parts (being mainly used in oil resistant rubber overshoes class) each other, and the bonding between itself and fabric must use the non-polar rubbers such as neoprene latex to bond, guarantee finished product sticking power index; Three, usual poor processability in the mixing production process of neoprene latex, time mixing, heat-dissipating amount is large, quick heating, and easy roll banding cylinder, easily burns; Four, neoprene cement, especially the large packaging final prod neoprene cement of outsourcing, in use, usually can not disposablely use up because rhythm of production is connected the reason such as not smooth, rubber cement after parking, very easily scrap because char length loss is excessive, even if curability is normal, but usually all can cause change in concentration, concentration uprises, cause brush coating difficulty, and easily cause rubber cement particle, carry out punching as used solvent, thinner etc. and convert, easily cause again concentration on the low side, easily cause inside fabric after brush coating and thoroughly starch, both all affect finished appearance, cause quality product to lose.
Therefore, for the problems referred to above, need to improve traditional formula; to reduce its toxic, the health of protection operator, can improve again technological operation performance in process for processing simultaneously; simplify preparation technology and operation steps; improve processing and fabricating efficiency, sticking power between sizing material and fabric is improved to finished product, meet slurry, non-discoloring performance thoroughly simultaneously; and then improve the over-all properties of rubber cement; improve product qualified rate, reach energy-saving and cost-reducing object, save Financial cost.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of toxicity little, with fabric and sizing material or cross-linked rubber parts strong adhesion, warping strength long service life, moderate viscosity, hot sulfurization neoprene cement that processing safety is good and preparation method thereof.
A kind of hot sulfurization neoprene cement of the present invention, rubber cement raw material comprises following component by weight: neoprene latex 90 ~ 95 parts, domestic No. 1 smoked sheet 5 ~ 10 parts, promotor 0.8 ~ 1 part, indirect process zinc oxide 4-6 part, light magnesium oxide 5 ~ 10 parts, anti-aging agent 1-2 part, scorch retarder 0 ~ 0.2 part, white carbon black 8 ~ 10 parts, tackifier 3-7 part, mixed solvent 190 ~ 195 parts;
Further, rubber cement raw material comprises following component by weight: neoprene latex 90 ~ 95 parts, domestic No. 1 smoked sheet 5 ~ 10 parts, promotor 0.8 ~ 1 part, indirect process zinc oxide 5 parts, light magnesium oxide 5 ~ 10 parts, 1.5 parts, anti-aging agent, scorch retarder 0 ~ 0.2 part, white carbon black 8 ~ 10 parts, tackifier 5 parts, mixed solvent 192 ~ 193 parts;
Further, neoprene latex 93 parts, domestic No. 1 smoked sheet 8 parts, promotor 0.9 part, indirect process zinc oxide 5 parts, light magnesium oxide 7 parts, 1.5 parts, anti-aging agent, scorch retarder 0.1 part, white carbon black 9 parts, tackifier 5 parts, mixed solvent 193 parts;
Further, described mixed solvent is butylacetate and 120# oil miscible solvent compound, and described butylacetate and 120# solvent oil weight ratio are 3:2;
Further, described promotor is accelerant N A-22;
Further, described anti-aging agent is the mixture of antioxidant 2246 and antioxidant SP-C, and described antioxidant 2246 and antioxidant SP-C part by weight are 1:2;
Further, described scorch retarder is altax; Described tackifier are terpine resin.
The present invention also discloses the preparation method of hot sulfurization neoprene cement, comprises the following steps:
A. plasticate: by setting weight part, domestic No. 1 smoked sheet is added mill, carry out at roller temperature is 40 DEG C ~ 50 DEG C thin-pass plasticate to Wei Shi plasticity number be 0.30-0.38;
B. mixing: neoprene latex being dropped into roller temperature is that the mill of 30 DEG C ~ 40 DEG C is subject to hot pressing soft to making sizing material, then roll spacing is relaxed, neoprene latex after input pressure is soft, and the domestic No. 1 smoked sheet film that input has been plasticated makes its bag roller, after sizing material is smooth, once add light magnesium oxide by setting weight part, promotor, anti-aging agent, white carbon black, indirect process zinc oxide carry out mixing and make film;
C. glue slurry: add part mixed solvent before opening stirrer as end oil, then mixed sheet is added stirrer, then the tackifier slowly adding setting weight part continue to stir 4-6 hour, 1-3 hour is stirred in the continuation adding some residual mixed solvent again, shut down and check concentration for the first time, and adding residue mixed solvent, after accumulative churning time reaches 7-9 hour, pulp is scraped sample censorship and is checked concentration, obtains product;
Further, in step c, be 40 ± 2 ° of Be by the concentration of rubber cement that B detects after pulp, rubber cement temperature is 25 DEG C, and detecting just sulphur point T10 with vulkameter after scraping sample drying is 142 DEG C × 45 ± 5 seconds;
Further; the amount adding end oil before opening stirrer is 3/4 of mixed solvent total amount; the tackifier adding setting weight part continue stirring 5 hours; the half adding residue mixed solvent continues stirring 2 hours; shut down and check concentration for the first time; and add residue mixed solvent, accumulative churning time is 8 hours.
Beneficial effect of the present invention: adopt butylacetate and 120# solvent oil to make mixed solvent, better deliquescently reduce because using benzene series solvent to the larger toxicity made and bring operative employee in use procedure having neoprene latex simultaneously, the viscosity of Simultaneous Stabilization finished product rubber cement, regulates the glued membrane rate of drying after brush coating; Adopt neoprene latex to be applicable to shaping hot sulfurization produce and can directly drop into mixing production, simplify the operation of refining glue; Adopt domestic No. 1 smoked sheet and neoprene latex and use, when can reduce refining glue, neoprene latex roll banding, improves mixing action performance; Adopt light magnesium oxide respectively, indirect process zinc oxide is as the activator of neoprene latex and vulcanizing agent; Accelerant N A-22 is as neoprene latex; Adopt altax (2,2'-dithio-bis-benzothiazole) as the scorch retarder of neoprene latex; Anti-aging agent adopts antioxidant 2246 and antioxidant SP-C and use, to improve the thermo oxidative aging of neoprene latex, and warping strength performance; Tackifier adopt terpine resin, to improve the viscosity of finished product rubber cement; White carbon black, as the filler of neoprene latex, has again certain strengthening action, and simultaneously white carbon black is as transparent material, can not pollute product shoes upper outward appearance after sulfuration.Hot sulfurization neoprene cement toxicity of the present invention prepared by the present invention is little, good with fabric and sizing material or cross-linked rubber parts strong adhesion, warping strength long service life, moderate viscosity, processing safety, and is easy to brush coating operation, reduces mass defect, improves product qualified rate.
Embodiment
Hot sulfurization neoprene cement of the present invention, rubber cement raw material comprises following component by weight: neoprene latex 90 ~ 95 parts, domestic No. 1 smoked sheet 5 ~ 10 parts, promotor 0.8 ~ 1 part, indirect process zinc oxide 4-6 part, light magnesium oxide 5 ~ 10 parts, anti-aging agent 1-2 part, scorch retarder 0 ~ 0.2 part, white carbon black 8 ~ 10 parts, tackifier 3-7 part, mixed solvent 190 ~ 195 parts; Be preferably neoprene latex (CR1211).
Be preferably, rubber cement raw material comprises following component by weight: neoprene latex 90 ~ 95 parts, domestic No. 1 smoked sheet 5 ~ 10 parts, promotor 0.8 ~ 1 part, indirect process zinc oxide 5 parts, light magnesium oxide 5 ~ 10 parts, 1.5 parts, anti-aging agent, scorch retarder 0 ~ 0.2 part, white carbon black 8 ~ 10 parts, tackifier 5 parts, mixed solvent 192 ~ 193 parts.
The best is, neoprene latex 93 parts, domestic No. 1 smoked sheet 8 parts, promotor 0.9 part, indirect process zinc oxide 5 parts, light magnesium oxide 7 parts, 1.5 parts, anti-aging agent, scorch retarder 0.1 part, white carbon black 9 parts, tackifier 5 parts, mixed solvent 193 parts.
In the present embodiment, described mixed solvent is butylacetate and 120# oil miscible solvent compound, and described butylacetate and 120# solvent oil weight ratio are 3:2.
In the present embodiment, described promotor is accelerant N A-22.
In the present embodiment, described anti-aging agent is the mixture of antioxidant 2246 and antioxidant SP-C, and described antioxidant 2246 and antioxidant SP-C weight ratio are preferably 1:2.
In the present embodiment, described scorch retarder is altax (2,2'-dithio-bis-benzothiazole), anti-scorch for neoprene latex; Described tackifier are terpine resin.
The present invention also discloses the preparation method of hot sulfurization neoprene cement, comprises the following steps:
A. plasticate: by setting weight part, domestic No. 1 smoked sheet is added mill, carry out at roller temperature is 40 DEG C ~ 50 DEG C thin-pass plasticate to Wei Shi plasticity number be 0.30-0.38;
B. mixing: neoprene latex being dropped into roller temperature is that the mill of 30 DEG C ~ 40 DEG C is subject to hot pressing soft to making sizing material, then roll spacing is relaxed, neoprene latex after input pressure is soft, and the domestic No. 1 smoked sheet film that input has been plasticated makes its bag roller, after sizing material is smooth, once add light magnesium oxide by setting weight part, promotor, anti-aging agent, white carbon black, indirect process zinc oxide carry out mixing and make film;
C. glue slurry: add part mixed solvent before opening stirrer as end oil, then mixed sheet is added stirrer, then the tackifier slowly adding setting weight part continue to stir 4-6 hour, 1-3 hour is stirred in the continuation adding some residual mixed solvent again, shut down and check concentration for the first time, and adding residue mixed solvent, after accumulative churning time reaches 7-9 hour, pulp is scraped sample censorship and is checked concentration, obtains product;
In the present embodiment, in step c, be 40 ± 2 ° of Be by the concentration of rubber cement that B detects after pulp, (rubber cement temperature is 25 DEG C), detecting just sulphur point T10 with vulkameter after scraping sample drying is 142 DEG C × 45 ± 5 seconds;
In the present embodiment; the amount adding end oil before opening stirrer is 3/4 of mixed solvent total amount; the tackifier adding setting weight part continue stirring 5 hours; the half adding residue mixed solvent continues stirring 2 hours; shut down and check concentration for the first time; and add residue mixed solvent, accumulative churning time is 8 hours.
Below by specific embodiment, the present invention is further elaborated.
Embodiment one
The hot sulfurization neoprene cement of the present embodiment, rubber cement raw material comprises following component by weight: neoprene latex 93 parts, domestic No. 1 smoked sheet 8 parts, promotor 0.9 part, indirect process zinc oxide 5 parts, light magnesium oxide 7 parts, 1.5 parts, anti-aging agent, scorch retarder 0.1 part, white carbon black 9 parts, tackifier 5 parts, mixed solvent 193 parts.
In the present embodiment, described mixed solvent is butylacetate and 120# oil miscible solvent compound, and described butylacetate and 120# solvent oil weight ratio are 3:2.
In the present embodiment, described promotor is accelerant N A-22.
In the present embodiment, described anti-aging agent is the mixture of antioxidant 2246 and antioxidant SP-C, described antioxidant 2246 and antioxidant SP-C weight ratio 1:2.
In the present embodiment, described scorch retarder is altax (2,2'-dithio-bis-benzothiazole), anti-scorch for neoprene latex; Described tackifier are terpine resin.
The preparation method of the present embodiment:
(1) plasticate:
First domestic No. 1 smoked sheet is cut into leg-of-mutton fritter, 5mm-8mm is transferred in the roll spacing of rubber breaker, drop into the domestic No. 1 smoked sheet block cut, treat that smoked sheet is broken into collodion silk, send mill to plasticate;
Thin-pass method of plasticating is used to plasticate to domestic No. 1 smoked sheet: to open water coolant and make roller temperature control at 45 DEG C, 0.5 ~ 1.0mm is adjusted in the roll spacing of mill, drops into domestic No. 1 smoked sheet collodion silk, carry out thin-pass to plasticate, use fan to cool sizing material during thin-pass, after thin-pass 3 times, relaxing roll spacing is 5mm-8mm, drop into through thin-pass domestic No. 1 smoked sheet and after bag roller, left and right cutter 2 times, after sizing material is smooth, blend glue stuff is also broken into film by lower detection sample, place, stand-by, place 9 hours; The plasticity number of plasticating (Wei Shi plasticity number) of the domestic No. 1 smoked sheet film that lower sample detects is 0.30-0.38.
(only plasticate to domestic No. 1 smoked sheet, neoprene latex (CR1211) is not plasticated)
(2) prepare burden:
Light magnesium oxide weighs separately and must seal preservation, prevents from making moist, packs separately after batching, to mixing use after batching, and 2 hours shelf-times;
Promotor, anti-aging agent are weighed respectively, and mixes rear loading one containers for future use;
Indirect process zinc oxide is weighed separately, loads a containers for future use;
Weigh in white carbon black separately, load a containers for future use;
Tackifier are carried out pulverizing preparing burden again, loads a containers for future use;
Butylacetate and 120# solvent oil are weighed by weight proportion respectively, and mixes rear loading one containers for future use;
(3) mixing:
Mill is used to carry out mixing, opening water coolant makes roller temperature control at 35 DEG C, 3 ~ 4mm is adjusted in the roll spacing of mill, drop into neoprene latex (CR1211) by 4 times, sizing material is made to be subject to hot pressing soft, relaxing roll spacing is 5mm ~ 6mm, drop into the soft rear neoprene latex (CR1211) of pressure, and the domestic No. 1 smoked sheet film that input has been plasticated makes its bag roller, after sizing material is smooth, first light magnesium oxide is added, add promotor again, anti-aging agent mixture, then coarse fodder white carbon black is added, finally add indirect process zinc oxide (not add when terpine resin is mixing, add again when slurrying).After dropping into each powder time mixing, all need left and right cutter 4 times, and clean powder, after before palpus, a kind of powder is suffered all, just can add lower a kind of powder, after all powders are suffered all, then play triangle bag and turn refining 2 ~ 3 times, 3 ~ 4mm is adjusted in the roll spacing of mill, slice, cooling, places, stand-by, 10 hours storage periods of rubber unvulcanizate.
(4) glue slurry
Before glue slurry, use slicing machine that cooled mixed sheet is cut into fritter, specification is about 5 × 80 × 100mm; Add part mixed solvent before opening stirrer as end oil, the amount of end oil is about 3/4 of mixed solvent total amount; Start stirrer, slowly add load weighted mixed sheet, must guard against bulk and add; After mixed sheet adds, more slowly add the rear load weighted tackifier of pulverizing; Tackifier add in solvent after film drops into solvent when making rubber cement again.
Should open the cooling of cooling water mixer summer, control to stir room temp and be no more than 40 DEG C, in order to avoid cause rubber cement to heat up too high and self-vulcanizing, winter is then contrary, forbids out water coolant, is convenient to film in mixed solvent dissolve; Stir 5 hours, after film all batters down, add second time solvent (half of residual solvent); Stir 2 hours again, shut down and check concentration for the first time, and adding residue mixed solvent, after accumulative churning time reaches 8 hours, pulp is scraped sample censorship and is checked concentration, obtains product.Be 40 ± 2 ° of Be (rubber cement temperature is 25 DEG C) by the concentration of rubber cement that B detects after pulp, detecting just sulphur point T10 with vulkameter after scraping sample drying is 142 DEG C × 45 ± 5 seconds.
Embodiment two
The hot sulfurization neoprene cement of the present embodiment, rubber cement raw material comprises following component by weight: neoprene latex 95 parts, domestic No. 1 smoked sheet 5 parts, promotor 0.9 part, indirect process zinc oxide 5 parts, light magnesium oxide 8 parts, 1.5 parts, anti-aging agent, scorch retarder 0.2 part, white carbon black 8 parts, tackifier 5 parts, mixed solvent 193.05 parts.
In the present embodiment, described mixed solvent is butylacetate and 120# oil miscible solvent compound, and described butylacetate and 120# solvent oil weight ratio are 3:2.
In the present embodiment, described promotor is accelerant N A-22.
In the present embodiment, described anti-aging agent is the mixture of antioxidant 2246 and antioxidant SP-C, and described antioxidant 2246 and antioxidant SP-C weight ratio are preferably 1:2.
In the present embodiment, described scorch retarder is altax (2,2'-dithio-bis-benzothiazole), anti-scorch for neoprene latex; Described tackifier are terpine resin.
The preparation method of the present embodiment is with embodiment one.
Embodiment three
The hot sulfurization neoprene cement of the present embodiment, rubber cement raw material comprises following component by weight: neoprene latex 95 parts, domestic No. 1 smoked sheet 5 parts, promotor 0.9 part, indirect process zinc oxide 5 parts, light magnesium oxide 8 parts, 1.5 parts, anti-aging agent, scorch retarder 0.2 part, white carbon black 8 parts, tackifier 5 parts, mixed solvent 193.05 parts.
In the present embodiment, described mixed solvent is butylacetate and 120# oil miscible solvent compound, and described butylacetate and 120# solvent oil weight ratio are 3:2.
In the present embodiment, described promotor is accelerant N A-22.
In the present embodiment, described anti-aging agent is the mixture of antioxidant 2246 and antioxidant SP-C, and described antioxidant 2246 and antioxidant SP-C weight ratio are preferably 1:2.
In the present embodiment, described scorch retarder is altax (2,2'-dithio-bis-benzothiazole), anti-scorch for neoprene latex; Described tackifier are terpine resin.
The preparation method of the present embodiment is with embodiment one
Embodiment four
The hot sulfurization neoprene cement of the present embodiment, rubber cement raw material comprises following component by weight: neoprene latex 90 parts, domestic No. 1 smoked sheet 10 parts, promotor 0.8 part, indirect process zinc oxide 5 parts, light magnesium oxide 6 parts, 1.5 parts, anti-aging agent, white carbon black 10 parts, tackifier 5 parts, mixed solvent 192.45 parts.
In the present embodiment, described mixed solvent is butylacetate and 120# oil miscible solvent compound, and described butylacetate and 120# solvent oil weight ratio are 3:2.
In the present embodiment, described promotor is accelerant N A-22.
In the present embodiment, described anti-aging agent is the mixture of antioxidant 2246 and antioxidant SP-C, and described antioxidant 2246 and antioxidant SP-C weight ratio are preferably 1:2.
In the present embodiment, described scorch retarder is altax (2,2'-dithio-bis-benzothiazole), anti-scorch for neoprene latex; Described tackifier are terpine resin.
The preparation method of the present embodiment:
(1) plasticate:
First domestic No. 1 smoked sheet is cut into leg-of-mutton fritter, 5mm-8mm is transferred in the roll spacing of rubber breaker, drop into the domestic No. 1 smoked sheet block cut, treat that smoked sheet is broken into collodion silk, send mill to plasticate;
Thin-pass method of plasticating is used to plasticate to domestic No. 1 smoked sheet: to open water coolant and make roller temperature control at 40 DEG C, 0.5 ~ 1.0mm is adjusted in the roll spacing of mill, drop into domestic No. 1 smoked sheet collodion silk, carry out thin-pass to plasticate, fan is used to cool sizing material during thin-pass, after thin-pass 3 times, relaxing roll spacing is 5mm-8mm, drop into through thin-pass domestic No. 1 smoked sheet and after bag roller, left and right cutter 2 times, after sizing material is smooth, blend glue stuff is also broken into film by lower detection sample, place, stand-by, 11 hours storage periods; The plasticity number of plasticating (Wei Shi plasticity number) of the domestic No. 1 smoked sheet film that lower sample detects is 0.30-0.38.
(only plasticate to domestic No. 1 smoked sheet, neoprene latex (CR1211) is not plasticated)
(2) prepare burden:
Light magnesium oxide weighs separately and must seal preservation, prevents from making moist, packs separately after batching, to mixing use after batching, and 3 hours shelf-times;
Promotor, anti-aging agent are weighed respectively, and mixes rear loading one containers for future use;
Indirect process zinc oxide is weighed separately, loads a containers for future use;
Weigh in white carbon black separately, load a containers for future use;
First terpine resin carries out pulverizing preparing burden again, loads a containers for future use;
Butylacetate and 120# solvent oil weigh by weight proportion respectively, and mix rear loading one containers for future use;
(3) mixing:
Mill is used to carry out mixing, opening water coolant makes roller temperature control at 30 DEG C, 3 ~ 4mm is adjusted in the roll spacing of mill, drop into neoprene latex (CR1211) by 4 times, sizing material is made to be subject to hot pressing soft, relaxing roll spacing is 5mm ~ 6mm, drop into the soft rear neoprene latex (CR1211) of pressure, and the domestic No. 1 smoked sheet film that input has been plasticated makes its bag roller, after sizing material is smooth, first light magnesium oxide is added, add promotor again, anti-aging agent mixture, then coarse fodder white carbon black is added, finally add indirect process zinc oxide (not add when terpine resin is mixing, add again when slurrying).After dropping into each powder time mixing, all need left and right cutter 4 times, and clean powder, after before palpus, a kind of powder is suffered all, just can add lower a kind of powder, after all powders are suffered all, then play triangle bag and turn refining 2 ~ 3 times, 3 ~ 4mm is adjusted in the roll spacing of mill, slice, cooling, places, stand-by, rubber unvulcanizate is less than 12 hours storage period.
(4) glue slurry
Before glue slurry, use slicing machine that cooled mixed sheet is cut into fritter, specification is about 5 × 80 × 100mm; Add part mixed solvent before opening stirrer as end oil, the amount of end oil is about 3/4 of mixed solvent total amount; Start stirrer, slowly add load weighted mixed sheet, must guard against bulk and add; After mixed sheet adds, more slowly add the rear load weighted tackifier of pulverizing; Tackifier add in solvent after film drops into solvent when making rubber cement again.
Should open the cooling of cooling water mixer summer, control to stir room temp and be no more than 40 DEG C, in order to avoid cause rubber cement to heat up too high and self-vulcanizing, winter is then contrary, forbids out water coolant, is convenient to film in mixed solvent dissolve; Stir 5 hours, after film all batters down, add second time solvent (part of residual solvent); Stir 2 hours again, shut down and check concentration for the first time, and adding residue mixed solvent, after accumulative churning time reaches 8 hours, pulp is scraped sample censorship and is checked concentration, obtains product.Be 40 ± 2 ° of Be (rubber cement temperature is 25 DEG C) by the concentration of rubber cement that B detects after pulp, detecting just sulphur point T10 with vulkameter after scraping sample drying is 142 DEG C × 45 ± 5 seconds.
Embodiment five
Neoprene latex 90 parts, domestic No. 1 smoked sheet 5 parts, promotor 0.8 part, indirect process zinc oxide 4 parts, light magnesium oxide 5 parts, 1 part, anti-aging agent, white carbon black 8 parts, tackifier 3 parts, mixed solvent 190 parts.
The preparation method of the present embodiment:
(1) plasticate:
First domestic No. 1 smoked sheet is cut into leg-of-mutton fritter, 5mm-8mm is transferred in the roll spacing of rubber breaker, drop into the domestic No. 1 smoked sheet block cut, treat that smoked sheet is broken into collodion silk, send mill to plasticate;
Thin-pass method of plasticating is used to plasticate to domestic No. 1 smoked sheet: to open water coolant and make roller temperature control at 40 DEG C ~ 50 DEG C, 0.5 ~ 1.0mm is adjusted in the roll spacing of mill, drop into domestic No. 1 smoked sheet collodion silk, carry out thin-pass to plasticate, fan is used to cool sizing material during thin-pass, after thin-pass 3 times, relaxing roll spacing is 5mm-8mm, drop into through thin-pass domestic No. 1 smoked sheet and after bag roller, left and right cutter 2 times, after sizing material is smooth, blend glue stuff is also broken into film by lower detection sample, place, stand-by, be greater than 8 hours storage period; The plasticity number of plasticating (Wei Shi plasticity number) of the domestic No. 1 smoked sheet film that lower sample detects is 0.30-0.38.
(only plasticate to domestic No. 1 smoked sheet, neoprene latex (CR1211) is not plasticated)
(2) prepare burden:
Light magnesium oxide weighs separately and must seal preservation, prevents from making moist, packs separately after batching, and to mixing use after batching, the shelf-time must not more than 4 hours;
Promotor, anti-aging agent are weighed respectively, and mixes rear loading one containers for future use;
Indirect process zinc oxide is weighed separately, loads a containers for future use;
Weigh in white carbon black separately, load a containers for future use;
First terpine resin carries out pulverizing preparing burden again, loads a containers for future use;
Butylacetate and 120# solvent oil weigh by weight proportion respectively, and mix rear loading one containers for future use;
(3) mixing:
Mill is used to carry out mixing, opening water coolant makes roller temperature control at 30 DEG C ~ 40 DEG C, 3 ~ 4mm is adjusted in the roll spacing of mill, drop into neoprene latex (CR1211) by 3 ~ 4 times, sizing material is made to be subject to hot pressing soft, relaxing roll spacing is 5mm ~ 6mm, drop into the soft rear neoprene latex (CR1211) of pressure, and the domestic No. 1 smoked sheet film that input has been plasticated makes its bag roller, after sizing material is smooth, first light magnesium oxide is added, add promotor again, anti-aging agent mixture, then coarse fodder white carbon black is added, finally add indirect process zinc oxide (not add when terpine resin is mixing, add again when slurrying).After dropping into each powder time mixing, all need left and right cutter 3 ~ 4 times, and clean powder, after before palpus, a kind of powder is suffered all, just can add lower a kind of powder, after all powders are suffered all, then play triangle bag and turn refining 2 ~ 3 times, 3 ~ 4mm is adjusted in the roll spacing of mill, slice, cooling, places, stand-by, rubber unvulcanizate is less than 12 hours storage period.
(4) glue slurry
Before glue slurry, use slicing machine that cooled mixed sheet is cut into fritter, specification is about 5 × 80 × 100mm; Add part mixed solvent before opening stirrer as end oil, the amount of end oil is about 3/4 of mixed solvent total amount; Start stirrer, slowly add load weighted mixed sheet, must guard against bulk and add; After mixed sheet adds, more slowly add the rear load weighted tackifier of pulverizing; Tackifier add in solvent after film drops into solvent when making rubber cement again.
Should open the cooling of cooling water mixer summer, control to stir room temp and be no more than 40 DEG C, in order to avoid cause rubber cement to heat up too high and self-vulcanizing, winter is then contrary, forbids out water coolant, is convenient to film in mixed solvent dissolve; Stir 5 hours, after film all batters down, add second time solvent (half of residual solvent); Stir 2 hours again, shut down and check concentration for the first time, and adding residue mixed solvent, after accumulative churning time reaches 8 hours, pulp is scraped sample censorship and is checked concentration, obtains product.Be 40 ± 2 ° of Be (rubber cement temperature is 25 DEG C) by the concentration of rubber cement that B detects after pulp, detecting just sulphur point T10 with vulkameter after scraping sample drying is 142 DEG C × 45 ± 5 seconds.
Embodiment six
Neoprene latex 95 parts, domestic No. 1 smoked sheet 10 parts, promotor 1 part, indirect process zinc oxide 6 parts, light magnesium oxide 10 parts, 2 parts, anti-aging agent, scorch retarder 0.15 part, white carbon black 10 parts, tackifier 7 parts, mixed solvent 195 parts.
In the present embodiment, described mixed solvent is butylacetate and 120# oil miscible solvent compound, and described butylacetate and 120# solvent oil weight ratio are 3:2.
In the present embodiment, described promotor is accelerant N A-22.
In the present embodiment, described anti-aging agent is the mixture of antioxidant 2246 and antioxidant SP-C, and described antioxidant 2246 and antioxidant SP-C weight ratio are preferably 1:2.
In the present embodiment, described scorch retarder is altax (2,2'-dithio-bis-benzothiazole), anti-scorch for neoprene latex; Described tackifier are terpine resin.
The preparation method of the present embodiment:
(1) plasticate:
First domestic No. 1 smoked sheet is cut into leg-of-mutton fritter, 5mm-8mm is transferred in the roll spacing of rubber breaker, drop into the domestic No. 1 smoked sheet block cut, treat that smoked sheet is broken into collodion silk, send mill to plasticate;
Thin-pass method of plasticating is used to plasticate to domestic No. 1 smoked sheet: to open water coolant and make roller temperature control at 40 DEG C ~ 50 DEG C, 0.5 ~ 1.0mm is adjusted in the roll spacing of mill, drop into domestic No. 1 smoked sheet collodion silk, carry out thin-pass to plasticate, fan is used to cool sizing material during thin-pass, after thin-pass 3 times, relaxing roll spacing is 5mm-8mm, drop into through thin-pass domestic No. 1 smoked sheet and after bag roller, left and right cutter 2 times, after sizing material is smooth, blend glue stuff is also broken into film by lower detection sample, place, stand-by, be greater than 8 hours storage period; The plasticity number of plasticating (Wei Shi plasticity number) of the domestic No. 1 smoked sheet film that lower sample detects is 0.30-0.38.
(only plasticate to domestic No. 1 smoked sheet, neoprene latex (CR1211) is not plasticated)
(2) prepare burden:
Light magnesium oxide weighs separately and must seal preservation, prevents from making moist, packs separately after batching, and to mixing use after batching, the shelf-time must not more than 4 hours;
Promotor, anti-aging agent are weighed respectively, and mixes rear loading one containers for future use;
Indirect process zinc oxide is weighed separately, loads a containers for future use;
Weigh in white carbon black separately, load a containers for future use;
First terpine resin carries out pulverizing preparing burden again, loads a containers for future use;
Butylacetate and 120# solvent oil weigh by weight proportion respectively, and mix rear loading one containers for future use;
(3) mixing:
Mill is used to carry out mixing, opening water coolant makes roller temperature control at 30 DEG C ~ 40 DEG C, 3 ~ 4mm is adjusted in the roll spacing of mill, drop into neoprene latex (CR1211) by 3 ~ 4 times, sizing material is made to be subject to hot pressing soft, relaxing roll spacing is 5mm ~ 6mm, drop into the soft rear neoprene latex (CR1211) of pressure, and the domestic No. 1 smoked sheet film that input has been plasticated makes its bag roller, after sizing material is smooth, first light magnesium oxide is added, add promotor again, anti-aging agent mixture, then coarse fodder white carbon black is added, finally add indirect process zinc oxide (not add when terpine resin is mixing, add again when slurrying).After dropping into each powder time mixing, all need left and right cutter 3 ~ 4 times, and clean powder, after before palpus, a kind of powder is suffered all, just can add lower a kind of powder, after all powders are suffered all, then play triangle bag and turn refining 2 ~ 3 times, 3 ~ 4mm is adjusted in the roll spacing of mill, slice, cooling, places, stand-by, rubber unvulcanizate is less than 12 hours storage period.
(4) glue slurry
Before glue slurry, use slicing machine that cooled mixed sheet is cut into fritter, specification is about 5 × 80 × 100mm; Add part mixed solvent before opening stirrer as end oil, the amount of end oil is about 3/4 of mixed solvent total amount; Start stirrer, slowly add load weighted mixed sheet, must guard against bulk and add; After mixed sheet adds, more slowly add the rear load weighted tackifier of pulverizing; Tackifier add in solvent after film drops into solvent when making rubber cement again.
Should open the cooling of cooling water mixer summer, control to stir room temp and be no more than 40 DEG C, in order to avoid cause rubber cement to heat up too high and self-vulcanizing, winter is then contrary, forbids out water coolant, is convenient to film in mixed solvent dissolve; Stir 5 hours, after film all batters down, add second time solvent (half of residual solvent); Stir 2 hours again, shut down and check concentration for the first time, and adding residue mixed solvent, after accumulative churning time reaches 8 hours, pulp is scraped sample censorship and is checked concentration, obtains product.Be 40 ± 2 ° of Be (rubber cement temperature is 25 DEG C) by the concentration of rubber cement that B detects after pulp, detecting just sulphur point T10 with vulkameter after scraping sample drying is 142 DEG C × 45 ± 5 seconds.
Embodiment seven
Rubber cement raw material comprises following component by weight: neoprene latex 90 parts, domestic No. 1 smoked sheet 5 parts, promotor 0.8 part, indirect process zinc oxide 5 parts, light magnesium oxide 5 parts, 1.5 parts, anti-aging agent, scorch retarder 0.2 part, white carbon black 8 parts, tackifier 5 parts, mixed solvent 192 parts.
Preparation method is with embodiment six
Embodiment eight
Rubber cement raw material comprises following component by weight: neoprene latex 95 parts, domestic No. 1 smoked sheet 10 parts, promotor 1 part, indirect process zinc oxide 5 parts, light magnesium oxide 10 parts, 1.5 parts, anti-aging agent, scorch retarder 0.1 part, white carbon black 10 parts, tackifier 5 parts, mixed solvent 195 parts.
(1) plasticate:
First domestic No. 1 smoked sheet is cut into leg-of-mutton fritter, 5mm-8mm is transferred in the roll spacing of rubber breaker, drop into the domestic No. 1 smoked sheet block cut, treat that smoked sheet is broken into collodion silk, send mill to plasticate;
Thin-pass method of plasticating is used to plasticate to domestic No. 1 smoked sheet: to open water coolant and make roller temperature control at 40 DEG C ~ 50 DEG C, 0.5 ~ 1.0mm is adjusted in the roll spacing of mill, drop into domestic No. 1 smoked sheet collodion silk, carry out thin-pass to plasticate, fan is used to cool sizing material during thin-pass, after thin-pass 3 times, relaxing roll spacing is 5mm-8mm, drop into through thin-pass domestic No. 1 smoked sheet and after bag roller, left and right cutter 2 times, after sizing material is smooth, blend glue stuff is also broken into film by lower detection sample, place, stand-by, be greater than 8 hours storage period; The plasticity number of plasticating (Wei Shi plasticity number) of the domestic No. 1 smoked sheet film that lower sample detects is 0.30-0.38.
(only plasticate to domestic No. 1 smoked sheet, neoprene latex (CR1211) is not plasticated)
(2) prepare burden:
Light magnesium oxide weighs separately and must seal preservation, prevents from making moist, packs separately after batching, and to mixing use after batching, the shelf-time must not more than 4 hours;
Promotor, anti-aging agent are weighed respectively, and mixes rear loading one containers for future use;
Indirect process zinc oxide is weighed separately, loads a containers for future use;
Weigh in white carbon black separately, load a containers for future use;
First terpine resin carries out pulverizing preparing burden again, loads a containers for future use;
Butylacetate and 120# solvent oil weigh by weight proportion respectively, and mix rear loading one containers for future use;
(3) mixing:
Mill is used to carry out mixing, opening water coolant makes roller temperature control at 30 DEG C ~ 40 DEG C, 3 ~ 4mm is adjusted in the roll spacing of mill, drop into neoprene latex (CR1211) by 3 ~ 4 times, sizing material is made to be subject to hot pressing soft, relaxing roll spacing is 5mm ~ 6mm, drop into the soft rear neoprene latex (CR1211) of pressure, and the domestic No. 1 smoked sheet film that input has been plasticated makes its bag roller, after sizing material is smooth, first light magnesium oxide is added, add promotor again, anti-aging agent mixture, then coarse fodder white carbon black is added, finally add indirect process zinc oxide (not add when terpine resin is mixing, add again when slurrying).After dropping into each powder time mixing, all need left and right cutter 3 ~ 4 times, and clean powder, after before palpus, a kind of powder is suffered all, just can add lower a kind of powder, after all powders are suffered all, then play triangle bag and turn refining 2 ~ 3 times, 3 ~ 4mm is adjusted in the roll spacing of mill, slice, cooling, places, stand-by, rubber unvulcanizate is less than 12 hours storage period.
(4) glue slurry
Before glue slurry, use slicing machine that cooled mixed sheet is cut into fritter, specification is about 5 × 80 × 100mm; Add part mixed solvent before opening stirrer as end oil, the amount of end oil is about 3/4 of mixed solvent total amount; Start stirrer, slowly add load weighted mixed sheet, must guard against bulk and add; After mixed sheet adds, more slowly add the rear load weighted tackifier of pulverizing; Tackifier add in solvent after film drops into solvent when making rubber cement again.
Should open the cooling of cooling water mixer summer, control to stir room temp and be no more than 40 DEG C, in order to avoid cause rubber cement to heat up too high and self-vulcanizing, winter is then contrary, forbids out water coolant, is convenient to film in mixed solvent dissolve; Stir 5 hours, after film all batters down, add second time solvent (half of residual solvent); Stir 2 hours again, shut down and check concentration for the first time, and adding residue mixed solvent, after accumulative churning time reaches 8 hours, pulp is scraped sample censorship and is checked concentration, obtains product.Be 40 ± 2 ° of Be (rubber cement temperature is 25 DEG C) by the concentration of rubber cement that B detects after pulp, detecting just sulphur point T10 with vulkameter after scraping sample drying is 142 DEG C × 45 ± 5 seconds.
Respectively detected result is carried out as following table to the finished product oil-resistant rubber boot made of the hot sulfurization neoprene cement of above-described embodiment and the finished product oil-resistant rubber boot physical and mechanical properties using outsourcing neoprene cement to make:
With fabric clinging power (n/cm)
With the finished product that hot sulfurization neoprene cement of the present invention makes ≥42.0
Use the finished product that outsourcing neoprene cement makes 22.5~27.0
Respectively 21 working days (Discontinuous manufacture) quality product statisticses are produced as following table to the finished product oil-resistant rubber boot made of this hot sulfurization neoprene cement and the finished product oil-resistant rubber boot using outsourcing neoprene cement to make:
Comprehensive qualified rate (%)
With the finished product that hot sulfurization neoprene cement of the present invention makes 99.3
Use the finished product that outsourcing neoprene cement makes 98.7
Produce micelle and liner lining in 21 working days (Discontinuous manufacture) substandard product mass defects to the finished product oil-resistant rubber boot made of this hot sulfurization neoprene cement and the finished product oil-resistant rubber boot using outsourcing neoprene cement to make respectively thoroughly to starch two problems to account for all mass defect ration statistics results as follows:
Table:
As can be seen from These parameters, use this hot sulfurization neoprene cement to reach and improve product shoes boots physicochemical property, strengthen sticking power between sizing material and fabric, and modest viscosity, be easy to brush coating operation, reduce micelle, thoroughly starch defect, improve final product quality qualification rate, this hot sulfurization neoprene cement manufacture craft is simple simultaneously, production cycle length, rubber cement can being organized to produce by matching with finished product rhythm of production progress, meeting service requirements.This hot sulfurization neoprene cement selects the non-benzene series organic solvent adopted, and reduces rubber cement toxic, is conducive to protecting making, using the relevant employee of rubber cement healthy.
In above-described embodiment, the optimum weight ratio of mixed solvent and sizing material (containing tackifier) is 3:2;
Antioxidant 2246 system white or creamy white crystals powder, fusing point 120-130 DEG C; Density 1.04-1.09, is dissolved in the organic solvents such as ethanol, acetone, benzene, sherwood oil, water insoluble; Slightly phenol taste; This product is nontoxic, and storage security is good; This product is placed for a long time in blush, but do not affect its oil product, rubber, plastics use in antioxygen prevent old performance;
Antioxidant SP-C is the pale powder that SP is adsorbed on mineral filler, and performance is completely identical with SP (styrenated phenol);
Accelerant N A-22 is Thiourea; Altax is 2,2'-dithio-bis-benzothiazole; Neoprene latex is preferably neoprene latex CR1211; Certainly, physico-chemical property also can be adopted similar to above-mentioned substance or same purpose can be played in the present invention and effect replaces above-mentioned substance with other materials realizing goal of the invention of the present invention.
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not departing from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.

Claims (10)

1. a hot sulfurization neoprene cement, it is characterized in that: rubber cement raw material comprises following component by weight: neoprene latex 90 ~ 95 parts, domestic No. 1 smoked sheet 5 ~ 10 parts, promotor 0.8 ~ 1 part, indirect process zinc oxide 4 ~ 6 parts, light magnesium oxide 5 ~ 10 parts, 1 ~ 2 part, anti-aging agent, scorch retarder 0 ~ 0.2 part, white carbon black 8 ~ 10 parts, tackifier 3 ~ 7 parts, mixed solvent 190 ~ 195 parts, described hot sulfurization neoprene cement is obtained by the preparation method comprised the following steps:
A. plasticate: by setting weight part, domestic No. 1 smoked sheet is added mill, carry out at roller temperature is 40 DEG C ~ 50 DEG C thin-pass plasticate to Wei Shi plasticity number be 0.30-0.38;
B. mixing: neoprene latex being dropped into roller temperature is that the mill of 30 DEG C ~ 40 DEG C is subject to hot pressing soft to making sizing material, then roll spacing is relaxed, neoprene latex after input pressure is soft, and the domestic No. 1 smoked sheet film that input has been plasticated makes its bag roller, after sizing material is smooth, once add light magnesium oxide by setting weight part, promotor, anti-aging agent, white carbon black, indirect process zinc oxide carry out mixing and make film;
C. glue slurry: add part mixed solvent before opening stirrer as end oil; then mixed sheet is added stirrer; then the tackifier slowly adding setting weight part continue to stir 4-6 hour; 1-3 hour is stirred in the continuation adding some residual mixed solvent again; shut down and check concentration for the first time, and adding residue mixed solvent, after accumulative churning time reaches 7-9 hour; pulp is scraped sample censorship and is checked concentration, obtains product.
2. hot sulfurization neoprene cement according to claim 1, is characterized in that: rubber cement raw material comprises following component by weight: neoprene latex 90 ~ 95 parts, domestic No. 1 smoked sheet 5 ~ 10 parts, promotor 0.8 ~ 1 part, indirect process zinc oxide 5 parts, light magnesium oxide 5 ~ 10 parts, 1.5 parts, anti-aging agent, scorch retarder 0 ~ 0.2 part, white carbon black 8 ~ 10 parts, tackifier 5 parts, mixed solvent 192 ~ 193 parts.
3. hot sulfurization neoprene cement according to claim 2, is characterized in that: rubber cement raw material comprises following component by weight: neoprene latex 93 parts, domestic No. 1 smoked sheet 8 parts, promotor 0.9 part, indirect process zinc oxide 5 parts, light magnesium oxide 7 parts, 1.5 parts, anti-aging agent, scorch retarder 0.1 part, white carbon black 9 parts, tackifier 5 parts, mixed solvent 193 parts.
4. the hot sulfurization neoprene cement according to the arbitrary claim of claim 1-3, is characterized in that: described mixed solvent is the mixture of butylacetate and 120# solvent oil, and described butylacetate and 120# solvent oil weight ratio are 3:2.
5. hot sulfurization neoprene cement according to claim 4, is characterized in that: described promotor is accelerant N A-22.
6. hot sulfurization neoprene cement according to claim 5, is characterized in that: described anti-aging agent is the mixture of antioxidant 2246 and antioxidant SP-C, and described antioxidant 2246 and antioxidant SP-C part by weight are 1:2.
7. hot sulfurization neoprene cement according to claim 6, is characterized in that: described scorch retarder is altax; Described tackifier are terpine resin.
8. a preparation method for hot sulfurization neoprene cement according to claim 1, is characterized in that: comprise the following steps:
A. plasticate: by setting weight part, domestic No. 1 smoked sheet is added mill, carry out at roller temperature is 40 DEG C ~ 50 DEG C thin-pass plasticate to Wei Shi plasticity number be 0.30-0.38;
B. mixing: neoprene latex being dropped into roller temperature is that the mill of 30 DEG C ~ 40 DEG C is subject to hot pressing soft to making sizing material, then roll spacing is relaxed, neoprene latex after input pressure is soft, and the domestic No. 1 smoked sheet film that input has been plasticated makes its bag roller, after sizing material is smooth, once add light magnesium oxide by setting weight part, promotor, anti-aging agent, white carbon black, indirect process zinc oxide carry out mixing and make film;
C. glue slurry: add part mixed solvent before opening stirrer as end oil; then mixed sheet is added stirrer; then the tackifier slowly adding setting weight part continue to stir 4-6 hour; 1-3 hour is stirred in the continuation adding some residual mixed solvent again; shut down and check concentration for the first time, and adding residue mixed solvent, after accumulative churning time reaches 7-9 hour; pulp is scraped sample censorship and is checked concentration, obtains product.
9. the preparation method of hot sulfurization neoprene cement according to claim 8, it is characterized in that: in step c, be 40 ± 2 ° of Be by the concentration of rubber cement that B detects after pulp, rubber cement temperature is 25 DEG C, and detecting just sulphur point T10 with vulkameter after scraping sample drying is 142 DEG C × 45 ± 5 seconds.
10. the preparation method of hot sulfurization neoprene cement according to claim 9; it is characterized in that: the amount adding end oil before opening stirrer is 3/4 of mixed solvent total amount; the tackifier adding setting weight part continue stirring 5 hours; the half adding residue mixed solvent continues stirring 2 hours; shut down and check concentration for the first time; and add residue mixed solvent, accumulative churning time is 8 hours.
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