CN103613868A - Novel vulcanization system-containing chlorinated polyethylene mixed rubber and processing technology - Google Patents
Novel vulcanization system-containing chlorinated polyethylene mixed rubber and processing technology Download PDFInfo
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- CN103613868A CN103613868A CN201310189997.5A CN201310189997A CN103613868A CN 103613868 A CN103613868 A CN 103613868A CN 201310189997 A CN201310189997 A CN 201310189997A CN 103613868 A CN103613868 A CN 103613868A
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
- B29B7/22—Component parts, details or accessories; Auxiliary operations
- B29B7/28—Component parts, details or accessories; Auxiliary operations for measuring, controlling or regulating, e.g. viscosity control
- B29B7/286—Component parts, details or accessories; Auxiliary operations for measuring, controlling or regulating, e.g. viscosity control measuring properties of the mixture, e.g. temperature, density
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
- B29B7/58—Component parts, details or accessories; Auxiliary operations
- B29B7/72—Measuring, controlling or regulating
- B29B7/726—Measuring properties of mixture, e.g. temperature or density
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- 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
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- 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
- C08K5/56—Organo-metallic compounds, i.e. organic compounds containing a metal-to-carbon bond
- C08K5/57—Organo-tin compounds
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- 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
- C08K2003/2206—Oxides; Hydroxides of metals of calcium, strontium or barium
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- 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
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
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- Engineering & Computer Science (AREA)
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Abstract
The invention provides novel vulcanization system-containing chlorinated polyethylene mixed rubber and a processing technology, and relates to a novel vulcanization system of chlorinated polyethylene rubber mixed rubber and a processing technology for the mixed rubber. The system is composed of, by weight, 100 parts of chlorinated polyethylene, 8-20 parts of light magnesium oxide, 3-9 parts of calcium hydroxide, 0-2 parts of methyl tin, 0-5 parts of mold releasing agents, 20-200 parts of reinforcing filling agents, 10-100 parts of plasticizers and 2-6 parts of vulcanization crosslinking systems. The technology process relates to the mixing temperature and the charging sequence, and the mixed rubber which is mixed uniformly and suitable for processing products is ensured. When the mixed rubber is compared with traditional products, the vulcanization speed is fast, and the vulcanized rubber has good mechanical properties. The mixed rubber has low cost compared with foreign products with the same effects.
Description
Technical field
The invention belongs to rubber processing, related is formula and the complete processing of chlorinated polyethylene rubber rubber unvulcanizate.
Background technology
Chlorinated polyethylene resin is a kind of novel synthetic materials, has a series of excellent properties.It is the good synthetic rubber of over-all properties, has very wide application field, has been widely used in the goods such as cable, electric wire, sebific duct, adhesive plaster, product of rubber and plastic, sealing material, flame-retardant conveyor belt, waterproof roll, film and various profiled materials.Chlorinatedpolyethylene can be regarded ethene, polyethylene and 1 as, the random copolymers of 2-Ethylene Dichloride, its molecular chain is saturated, polarity chlorine atom random distribution, because there is excellent physicals and chemical property, be widely used in machinery, electric power, chemical industry, building materials and mine industry.Chlorinated polyethylene rubber thermotolerance, resistance to ozone and weather-proof, be ageing-resistantly better than most rubber, oil-proofness is better than paracril (NBR), chloroprene rubber (CR), the ageing-resistant chlorosulphonation vinylchlorid (CSM) that is better than; The corrosion property such as acid-and base-resisting, salt, nontoxic, difficult combustion, without explosion hazard.
Up to the present, the sulfuration of chlorinated polyethylene rubber has been done to large quantity research both at home and abroad.Present domestic two kinds of vulcanization system peroxide vulcanizing systems and the thiourea curing system of mainly containing.During peroxide cure CPE rubber, easily produce bubble and very large smell, can not open vulcanization, the mechanical property of cross-linked rubber is bad; The vulcanization rate of thiourea curing system is slower, and the resistance toheat of cross-linked rubber is bad, and Rubber processing industry wishes to find the good vulcanizing agent of the good scorching quality of a kind of curability especially.Developed very early thiadiazoles derivative vulcanization system abroad, had the advantage of peroxide vulcanizing system and thiourea curing system concurrently, but its system chemical composition is underground, and expensive, domestic very few popularization.The analogous products thiadiazoles derivative vulcanization system that Yantai Thinking Finechem Technology Co., Ltd.'s independent research is produced can reach identical effect, and vulcanization rate is fast, and cross-linked rubber mechanical property is excellent, sulfurizing temperature range is wide, can open vulcanization, can substitute external product completely, and cost is relatively low.Chlorinated polyethylene rubber rubber unvulcanizate based on this is not promoted.
The patent CN101463168 A of Tianjin Penglingjiao Guan Co., Ltd has introduced the chlorinated polythylene rubber pipe formula that thiazole derivative is vulcanizing agent of take, related vulcanization system is from German vulcanizing agent TDD and vulcanization accelerator NC, application is sebific duct, related formulation cost is higher, and application is single.
The patent CN1002617944 A of Wuxi City Yuan Deng Cable Co., Ltd has introduced a kind of manufacture wind energy cable chlorinated polyethylene rubber and preparation method thereof, it is peroxide vulcanizing system that its formula relates to vulcanization system, and design mainly for wind energy cable, contained stablizer lead sulfate tribasic is domestic forbidding auxiliary agent, harmful in human body.
The patent CN102585390 A of Hengshui Xin Lu transportation equipment company limited has introduced a kind of formula and preparation technology of chlorinated polyethylene rubber waterstop, it is peroxide vulcanizing system that its formula relates to vulcanization system, and stablizer used is the product that lead salts is harmful to HUMAN HEALTH.
In the research > > of the < < CM Thiadiazole Curing System that the people such as Nie Jun, Wang Shengyuan delivered in June, 2005 on specialty elastomer goods magazine, research has illustrated the impact of Thiadiazole Curing System consumption proportion on chlorinated polyethylene rubber mechanical property, obtained the optimum amount of vulcanizing agent and promotor, but related vulcanizing agent and vulcanization accelerator are German product TDD and NC, from to the present invention relates to vulcanization system different, and cost is higher.
Through retrieval, both at home and abroad there are no take report and the research of domestic thiadiazole derivs objects system as vulcanization system production chlorinatedpolyethylene rubber unvulcanizate.
Summary of the invention
Drawback and deficiency for now conventional chlorinatedpolyethylene rubber unvulcanizate, the object of this invention is to provide a kind of chlorinatedpolyethylene rubber unvulcanizate that domestic thiadiazoles derivative is vulcanizing agent of take, curing time is short, and cured properties is good, and the more external peer-level rubber unvulcanizate of cost is low.
The present invention is that the technical scheme that realizes goal of the invention employing is, containing the chlorinatedpolyethylene rubber unvulcanizate formula of novel vulcanization system, described rubber unvulcanizate is to take rubber-type chlorinated polyethylene as base-material, by specific calendering process, produces, and key is that described formula is:
Chlorinatedpolyethylene 100
Light magnesium oxide 8-20
Calcium hydroxide 3-9
Methyl tin 0-2
Releasing agent 0-5
Reinforcing and filling system 20-200
Softening agent 10-100
Vulcanization crosslinking system 2-6
The invention still further relates to the complete processing of chlorinatedpolyethylene rubber unvulcanizate, key is that described complete processing can be mill blend or Banbury mixer blend:
(1) mill blending technology: first add chlorinated polyethylene rubber powder in mill, control mill temperature between 60-100 ℃, add softening agent, light magnesium oxide, calcium hydroxide and methyl tin, then reinforcing and filling system is added, add again releasing agent and domestic thiadiazoles derivative vulcanizing agent, after material feeding completes, turn roll spacing down, thin-pass for several times, slice is cooling, and promotor is joined in mixed sheet, after material feeding completes below at 50 ℃, for several times, slice is cooling for thin-pass.Early stage, mixing process can carry out in Banbury mixer.
(2) Banbury mixer blending technology: first add chlorinatedpolyethylene powder, control Banbury mixer temperature, at 100-140 ℃, carry out mixingly, after material is agglomerating, add the auxiliary material except promotor, after balance, depending on practical situation discharging, material slice in mill is cooling, and temperature adds promotor in the time of 40-80 ℃, mixing even, thin-pass 5-10 time, slice is cooling, packing.
In the above-mentioned formula of the chlorinatedpolyethylene rubber unvulcanizate containing novel vulcanization system: described rubber unvulcanizate base-material chlorinated polyethylene rubber is that cl content is the saturated chlorinated polyethylene rubber of 25%-45%.
In the above-mentioned chlorinatedpolyethylene rubber unvulcanizate formula containing novel vulcanization system: described reinforcing and filling system is a kind of in carbon black (except thermally oxidized black), light calcium carbonate, water-ground limestone, talcum powder, mica powder and white carbon black, or above two kinds or two or more strengthening agent share.
The reinforcing and filling system of the above-mentioned chlorinatedpolyethylene rubber unvulcanizate containing novel vulcanization system: when described reinforcing and filling system is white carbon black, should be equipped with the conditioning agent of its consumption 8%-15%, it is one or both or three kinds in trolamine, glycol ether, Macrogol 4000 that conditioning agent requires.
In the above-mentioned chlorinatedpolyethylene rubber unvulcanizate formula containing novel vulcanization system: described softening agent is a kind of in tri-n-butyl citrate, Octyl adipate (DOA), dioctyl sebacate (DOS), Uniflex DBS (DBS), dioctyl phthalate (DOP) (DOP), dibutyl phthalate (DBP), dioctyl azelate (DOZ), aromatic hydrocarbon oil (alkalescence), or above two kinds or two or more softening agent share.
In the above-mentioned chlorinatedpolyethylene rubber unvulcanizate formula containing novel vulcanization system: the consumption of described reinforcing and filling system, softening agent can regulate by product properties requirement, make the rubber unvulcanizate can be for the product of different performance requirement.
In above-mentioned chlorinatedpolyethylene rubber unvulcanizate formula: described stablizer is methyl tin.
In above-mentioned chlorinatedpolyethylene rubber unvulcanizate formula: described releasing agent is the mould 935P that gets profit, and applies in pressing.
In above-mentioned chlorinatedpolyethylene rubber unvulcanizate formula: described vulcanization system is the product of domestic thiadiazoles derivative vulcanizing agent and promotor ，Shi Yantai Thinking Finechem Technology Co., Ltd., requires consumption respectively between 1.5-4 part and between 0.5-1.5 part.
In the complete processing of above-mentioned chlorinatedpolyethylene rubber unvulcanizate: described control mill temperature is between 60-100 ℃, and its optimum temps is between 80-90 ℃.
In the complete processing of above-mentioned chlorinatedpolyethylene rubber unvulcanizate: described mixer mixing temperature is between 100-140 ℃, and its optimum temps is between 110-130 ℃.
Gained rubber unvulcanizate of the present invention can make the vulcanized article of excellent property, and according to the difference of reinforcement and filler and plasticizer consumption, the tensile strength of vulcanized article can reach 7-20MPa, and tensile yield is between 300%-800%.Because vulcanization system consumption is less, close with peroxide vulcanizing system cost, cured properties is more excellent, and curing time is shorter.Gained rubber unvulcanizate of the present invention, sulfurizing temperature range is wide, can open vulcanization, can adapt to multiple sulfuration process, be applicable to the manufacture of the multiclass products such as electric wire, sebific duct, sealing article, travelling belt, also can promote the development of rubber-type chlorinated polyethylene.
Embodiment
Embodiment 1
By formula
Chlorinatedpolyethylene 100
Light magnesium oxide 12
Calcium hydroxide 5
Methyl tin 0.5
Releasing agent 3
Carbon black 60
Light calcium carbonate 30
Softening agent 25
Domestic thiadiazoles derivative vulcanizing agent 2.5
Promotor 1
Prepare various starting material, when Banbury mixer temperature is 110 ℃ of left and right, add chlorinatedpolyethylene, methyl tin, magnesium oxide and calcium hydroxide, mixingly reinforcing and filling system and softening agent are added after evenly, then add releasing agent and vulcanizing agent, be blended into balance, discharging, in mill, thin-pass is 5 times, lower cooling, temperature is down to 50 ℃ and in mill, is added promotor when following, completely after material feeding, and thin-pass 5 times, lower, obtain required rubber unvulcanizate.
Embodiment 2
By formula
Chlorinatedpolyethylene 100
Light magnesium oxide 10
Calcium hydroxide 7
Methyl tin 0.5
Releasing agent 3
Carbon black 50
Light calcium carbonate 60
Softening agent 40
Domestic thiadiazoles derivative vulcanizing agent 2.5
Promotor 0.8
Prepare various starting material, when mill temperature is 80 ℃ of left and right, add chlorinatedpolyethylene, add methyl tin, magnesium oxide and calcium hydroxide after wrapping in flakes roller, mixingly charcoal reinforcing and filling system and softening agent are added after evenly, then add releasing agent and vulcanizing agent, abundant thin-pass 5 times after material feeding, lower is cooling, and temperature is down to 50 ℃ and in mill, is added promotor when following, completely after material feeding, thin-pass 8 times,, obtains required rubber unvulcanizate by lower.
Embodiment 3
By formula
Chlorinatedpolyethylene 100
Light magnesium oxide 10
Calcium hydroxide 6
Methyl tin 0.5
Releasing agent 3
Carbon black 40
Light calcium carbonate 80
Softening agent 58
Domestic thiadiazoles derivative vulcanizing agent 3
Promotor 1
Prepare various starting material, when Banbury mixer temperature is 120 ℃ of left and right, add chlorinatedpolyethylene, methyl tin, magnesium oxide and calcium hydroxide, mixingly reinforcing and filling system and softening agent are added after evenly, then add releasing agent and vulcanizing agent, be blended into balance, discharging, in mill, thin-pass is 5 times, lower cooling, temperature is down to 50 ℃ and in mill, is added promotor when following, completely after material feeding, and thin-pass 8 times, lower, obtain required rubber unvulcanizate.
Embodiment 4
By formula
Chlorinatedpolyethylene 100
Light magnesium oxide 12
Calcium hydroxide 6
Methyl tin 0.5
Releasing agent 3
Carbon black 20
Light calcium carbonate 32
Softening agent 25
Domestic thiadiazoles derivative vulcanizing agent 3
Promotor 1.2
Prepare various starting material, when mill temperature is 85 ℃ of left and right, add chlorinatedpolyethylene, add methyl tin, magnesium oxide and calcium hydroxide after wrapping in flakes roller, mixingly reinforcing and filling system and softening agent are added after evenly, then add vulcanizing agent, abundant thin-pass 8 times after material feeding, lower is cooling, and temperature is down to 50 ℃ and in mill, is added promotor when following, completely after material feeding, thin-pass 8 times,, obtains required rubber unvulcanizate by lower.
By the fill a prescription consumption of MR medium reinforcing infill system, softening agent of adjusting, can make the rubber unvulcanizate that is applicable to multiple product, be applied to the goods such as electric wire, sealing member, transport tape, sebific duct, in production of articles process, curing time is short, resulting product mechanical property is good, the excellent performance such as ageing-resistant, weather-proof, fire-retardant, can promote the application in chlorinated polyethylene rubber market to a certain extent, reduces the cost of part rubber item.
Claims (9)
1. contain the chlorinatedpolyethylene rubber unvulcanizate of novel vulcanization system, described rubber unvulcanizate is to take rubber-type chlorinated polyethylene as base-material, by specific calendering process, make, it is characterized in that: described rubber unvulcanizate formula is: 100 parts of chlorinated polyethylene rubbers, light magnesium oxide 8-20 part, calcium hydroxide 3-9 part, methyl tin 0-2 part, releasing agent 0-5 part, reinforcing filler 20-200 part, softening agent 10-100 part, vulcanization crosslinking system 2-6 part.
2. according to claim 1 containing the chlorinatedpolyethylene rubber unvulcanizate formula of novel vulcanization system, it is characterized in that: described rubber unvulcanizate base-material chlorinated polyethylene rubber is that cl content is the saturated chlorinated polyethylene rubber of 25%-45%.
3. containing the chlorinatedpolyethylene rubber unvulcanizate of novel vulcanization system, fill a prescription according to claim 1, it is characterized in that: described reinforcing and filling system is a kind of in carbon black (except thermally oxidized black), light calcium carbonate, water-ground limestone, talcum powder, mica powder and white carbon black, or above two kinds or two or more strengthening agent share.
4. the reinforcing and filling system of rubber unvulcanizate according to claim 3, is characterized in that: while using white carbon black, should be equipped with the conditioning agent of its consumption 8%-15%, it is one or both or three kinds in trolamine, glycol ether, Macrogol 4000 that conditioning agent requires.
5. described in claim 1, the chlorinatedpolyethylene rubber unvulcanizate containing novel vulcanization system is filled a prescription, it is characterized in that: described softening agent is a kind of in tri-n-butyl citrate, Octyl adipate (DOA), dioctyl sebacate (DOS), Uniflex DBS (DBS), dioctyl phthalate (DOP) (DOP), dibutyl phthalate (DBP), dioctyl azelate (DOZ), aromatic hydrocarbon oil (alkalescence), or above two kinds or two or more softening agent share.
6. described in claim 1, the chlorinatedpolyethylene rubber unvulcanizate containing novel vulcanization system is filled a prescription, it is characterized in that: described vulcanization system is domestic thiadiazoles derivative vulcanizing agent and promotor, be the product of Yantai Thinking Finechem Technology Co., Ltd., require consumption respectively between 1.5-4 part and between 0.5-1.5 part.
7. described in claim 1, contain the chlorinatedpolyethylene rubber unvulcanizate of novel vulcanization system, it is characterized in that: the preparation technology of rubber unvulcanizate is mill blend or Banbury mixer blend.
8. described in claim 6, contain the mill blending technology of the chlorinatedpolyethylene rubber unvulcanizate of novel vulcanization system, it is characterized in that: first in mill, add chlorinatedpolyethylene powder, control mill temperature between 60-100 ℃, polyethylene rubber to be chlorinated becomes transparent colloid, add softening agent, light magnesium oxide, calcium hydroxide and methyl tin, then reinforcing and filling system is added, add again releasing agent and domestic thiadiazoles derivative vulcanizing agent, after material feeding completes, turn roll spacing down, thin-pass 5-10 time, slice is cooling, promotor is joined in mixed sheet at 40-80 ℃, after material feeding completes, thin-pass 5-10 time, slice is cooling, packing.
9. the Banbury mixer refining machine blending technology that contains the chlorinatedpolyethylene rubber unvulcanizate of novel vulcanization system described in claim 6, is characterized in that: first add chlorinatedpolyethylene powder, control Banbury mixer temperature, at 100-140 ℃, carry out mixing, after material is agglomerating, add the auxiliary material except promotor, after balance, depending on practical situation discharging, material slice in mill is cooling, temperature adds promotor in the time of 40-80 ℃, mixing even, thin-pass 5-10 time, slice is cooling, packing.
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Cited By (7)
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| CN105385052A (en) * | 2015-09-23 | 2016-03-09 | 南京七四二五橡塑有限责任公司 | Rubber composition of low-temperature resistant environmentally-friendly chlorinated polyethylene and preparation method thereof |
| CN105924812A (en) * | 2016-05-23 | 2016-09-07 | 无锡市嘉邦电力管道厂 | Cable insulation material |
| CN106496827A (en) * | 2016-11-08 | 2017-03-15 | 福建梭罗复合材料研究有限公司 | A kind of polyester fiber modified chlorinated polyethylene specific rubber and preparation method thereof |
| CN108410075A (en) * | 2018-03-13 | 2018-08-17 | 杭州科利化工股份有限公司 | A kind of chlorinated polyethylene rubber combination new material and preparation method thereof |
| CN110713668A (en) * | 2018-07-13 | 2020-01-21 | 浙江大学 | Halogenated polyethylene rubber and processing method thereof |
| CN113999463A (en) * | 2021-11-25 | 2022-02-01 | 刘现海 | Chlorinated polyethylene and polyethylene blending modified pipe and preparation method thereof |
| CN114672102A (en) * | 2022-05-26 | 2022-06-28 | 中裕铁信交通科技股份有限公司 | Hydrogen sulfide corrosion resistant rubber waterstop and preparation method thereof |
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| CN110713668A (en) * | 2018-07-13 | 2020-01-21 | 浙江大学 | Halogenated polyethylene rubber and processing method thereof |
| CN113999463A (en) * | 2021-11-25 | 2022-02-01 | 刘现海 | Chlorinated polyethylene and polyethylene blending modified pipe and preparation method thereof |
| CN113999463B (en) * | 2021-11-25 | 2023-01-17 | 刘现海 | Chlorinated polyethylene and polyethylene blending modified pipe and preparation method thereof |
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