CN105111525A - Production method of anti-ozone high-performance natural rubber - Google Patents
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Abstract
The invention belongs to the field of natural rubber production technology, and relates to a production method of anti-ozone high-performance natural rubber. The production method comprises the steps of taking fresh natural rubber latex of a natural rubber strain, which is suitable for binding with protein, adding alkaline protease and adopting a freezing method to freeze the fresh rubber latex, so as to obtain flocculation glue; curdling and curing the flocculation glue to obtain a curd or a sheet rubber; laminating and dewatering, washing, pelleting, and pressing to obtain a rubber sheet; hanging and drying the rubber sheet, pelleting, drying and obtaining an anti-ozone high-performance natural rubber product. The production method provided by the invention is simple in production process and low in production cost, and each step adopts the process and the method having minimum damage on a rubber molecular chain, the nitrogen content is controlled, the protein having an important effect on ozone resistance and ageing resistance is retained, micro orientation of a local molecular chain is formed, the ozone resistance and high performance of the product are kept, the product quality is good, the production recovery is high, the production process is green and environment friendly, and the production is economical and efficient.
Description
Technical field
The invention belongs to natural rubber glue technical field, relate to a kind of production method of natural rubber, specifically a kind of production method of resistance to ozone high-property natural rubber.
Background technology
Natural rubber latex is except containing except rubber hydrocarbon and water; also containing non-rubber substances such as a large amount of protein, lipoid, organic acid and carbohydrates; because the rubber particles in natural rubber latex is subject to the electrostatic double layer protection of the hydrophilic substance such as protein and lipoid formation; natural rubber latex is made to keep stable colloidal state; when natural rubber latex microbial contamination; or add acid, inorganic salt, or in the situations such as heating, freezing, radiation, natural rubber latex all can be made to lose stable and solidify or gelling.At present, natural latex coargulation method is chemical method, biological process and physics freezing method mainly: one, chemical method, and the peptizer namely adding such as acid, salt, dewatering agent and so on makes latex coagulation; Two, biological process, namely utilizes the effect of microorganism original or additional in latex or enzyme to make latex coagulation; Three, physics freezing method, namely utilizes physical method as adopted the method for microwave radiation or heating, coagulation by mechanical stirring natural rubber latex.
Natural rubber latex is called plantation gel at the glue that plantation natural coagulation obtains, and mainly contains: glue cup lump, micelle, tree lace etc.; Natural rubber latex after artificial coagulation through compressing tablet, park the film that dehydration obtains and be called sheet rubber.Due to plantation gel, sheet rubber etc., often foreign matter content is high, after needing fully washing, is processed into standard rubber product through the operation such as granulation, drying.
The main pattern adopting concentrated processing of natural rubber processing of China, namely adds ammonia and makes preservatives, then transport latex back source mill concentrated processing in the fresh latex of plantation collection.It is that acid adding utilizes sour coagulum for neutralization of ammonia in fresh latex that the mode of factory's concentrated processing mainly contains two kinds: one, the grumeleuse after solidifying through crumpling, washing, granulation, dry post-treatment become standard rubber product; Two is that nature rubber latex obtains revertex after centrifugal concentrating is separated and glue is clear, and revertex is stabilized is processed into revertex with slaking.
At present, the standard natural rubber production assay solid through acid cure shows, the performance of its pure glue formula of most standard glue product is tensile strength is 19.6 ~ 20.5MPa, heatproof air aging performance is lower, resistance to ozone cracking can be 30 ~ 50 minutes, and mooney viscosity is about 60 ~ 70, plasticity initial value P
0between 30 ~ 40, PRI is between 65 ~ 80; The performance of its pure glue formula of standard rubber that most of sheet rubber is produced to be tensile strength be 20 ~ 22MPa, heatproof air aging performance are lower, and resistance to ozone cracking can be 40 ~ 60 minutes, and mooney viscosity is about 65 ~ 75, plasticity initial value P
0between 35 ~ 40, PRI is between 70 ~ 80.Above-mentioned two kinds of standard rubber products are all difficult to use in the high performance aircraft tyre of the resistance to ozone of production requirement and other high quality natural rubber products.Therefore, obtain resistance to ozone high-property natural rubber by suitable production technique and production method to be significant.
Current research shows: the performance of natural rubber, except by except the rubber chain structure influence of natural rubber, is also subject to the impact of nonrubber component and the impact of complete processing and condition.The molecular structure of natural rubber comprises: the molecular size range of rubber hydrocarbon-polyisoprene and molecular weight distribution.Nonrubber component mainly comprises: the molten thing of protein, lipoid, acetone, inorganic salt etc., nonrubber component total amount is about 3 ~ 5%.Complete processing and condition comprise: the degree of solidifying (solidification mode and consumption), compressing tablet, dehydration, washing and granulation of the early stage preservation (kind of preservatives and consumption) of fresh latex, latex; Dry condition (drying temperature, time and atmospheric moisture, flow).Affect in rubber performance and conforming factor, some factor is uncontrollable (as weather, season, soil etc.), some factor is mainly considered also to be difficult to control (strain, tapping system, fertilising etc. as gum) from Growth and yield angle, the most effective and the most feasible control and to obtain the high performance production method of resistance to ozone be control to the course of processing.
In the standard rubbers production technique that the fresh latex adopting ammonia to preserve uses acid to solidify natural rubber latex, residual ammonia can affect heatproof air aging performance and the resistance to ozone cracking energy of product with acid, and mechanical property reduces.Suitable compressing tablet, wash, crumple technique and can dewater and clean impurity and the material such as acid, ammonia, but excessive fragmentation, tear and can make molecular breakdown and the mechanical property injuring product.Kinds of protein in natural rubber mainly contains: α ball river flowing from Guizhou Province through Hunan into Dongting Lake albumen, rubber river flowing from Guizhou Province through Hunan into Dongting Lake albumen, basic protein and fibrous protein.Albumen mass-energy reduces the activation energy of sulfuration, promotes the vulcanization of rubber; The impact of difference on sulfuration of protein kind is variant, and meanwhile, the associated proteins that protein adsorption is formed on natural rubber molecular chain can improve heat-resisting oxygen and ozone ageing performance, and wherein, associated proteins is occupied an leading position with rubber river flowing from Guizhou Province through Hunan into Dongting Lake albumen; But protein is too much, vulcanization rate is unfavorable for producing too soon, and easy mildew, heat generation is high; The mensuration of protein content is calculated by the amino acid whose nitrogen content detected in protein.Therefore, the kinds of protein be applicable to and content can keep the ozone resistance of natural rubber.
The control of drying process is the key keeping resistance to ozone and obtain premium quality product, temperature is too high can make molecular chain degradation by havoc rubber molecular chain, and make the non-rubber substance on molecular chain be subject to heat collapse, product mechanical property and aging resistance and ozone resistance are reduced; Temperature is oversize for too low time of drying, also easily mildew, the phenomenon such as half-cooked.
Summary of the invention
The object of this invention is to provide a kind of production method of resistance to ozone high-property natural rubber, choose the natural rubber strain with suitable binding protein, adopt and minimum processing condition and method is destroyed to rubber molecular chain, nitrogen content is controlled in certain scope by Sumizyme MP freezing method, guarantee the protein content in rubber, guarantee ozone resistance, the lacing film drying of controllable temperature and humidity is utilized to make rubber molecular chain be subject to washing fragmentation, broken molecule chain is made again to recover after tearing, strict control drying temperature, make the non-rubber substance that rubber does not destroy rubber molecular chain as much as possible in drying process and shields to molecular chain, maintain resistance to ozone and the high-performance of product, production technique is easy, good product quality, the production rate of recovery is high, production process environmental protection, production economy is efficient.
The technology used in the present invention principle: the natural rubber latex choosing the suitable natural rubber strain of associated proteins, the rubber pig obtained by Sumizyme MP freezing method makes raw material, abundant foam washing after fully washing and be pressed into film, the acid that removing is residual, the materials such as ammonia, molecular chain is made to be subject to washing fragmentation by the abundant lacing film of kiln of controllable temperature and humidity, recover again after tearing, by strictly controlling lacing film drying temperature, make the non-rubber substance that rubber does not destroy rubber molecular chain as much as possible in drying process and shields to molecular chain, product is made to keep resistance to ozone and high-performance.
The technical solution adopted in the present invention is:
A production method for resistance to ozone high-property natural rubber, its concrete steps are as follows:
1, get drc and be 8 ~ 62% and the fresh natural rubber latex of natural rubber strain that the associated proteins of interpolation less than 0.05% ammonia is suitable by weight percentage, adding Sumizyme MP adopts freezing method to solidify fresh latex and obtain flocculent gel, its Control of Nitrogen Content (utilizes Sumizyme MP to decompose glue protein of milk 0.15 ~ 0.35%, make breaks down proteins become amino acid dissolve in water, in washing process, remove the nitrogen content reduced in latex); Flocculent gel being obtained grumeleuse or sheet rubber through solidifying with slaking, through ironed dehydration, washing, be pressed into the film that thickness is 2 ~ 15mm, guaranteeing that film does not rupture in lacing film process, the micro orientation that rubber molecule chain formation is certain can be made, and can be on time dry on request.Described associated proteins is suitable refers to that in fresh latex, rubber river flowing from Guizhou Province through Hunan into Dongting Lake albumen accounts for 10 ~ 40% of Tot Prot.
The strain that the natural rubber strain that described associated proteins is suitable comprises PRIM600, heat grinds 7-33-97, heat grinds 879, heat grinds the natural rubbers such as 72059 or PR107.
Described Sumizyme MP refers to that enzyme activity is greater than 6KPPU/g in the basic conditions, and total plate count is less than 10000/G.
2, by film loft dried, control temperature is 15 ~ 120 DEG C, and the loft dried time is 1 ~ 15 day.
3, the film through loft dried is carried out granulation, drying can obtain resistance to ozone high-property natural rubber product.
The present invention chooses the natural rubber latex of the suitable natural rubber strain of associated proteins, Sumizyme MP freezing method is adopted to make Control of Nitrogen Content 0.15 ~ 0.35%, the while of utilizing lacing film drying (film loft dried) dewatered, make rubber molecular chain in washing, granulation process is broken, recover again after tearing, and make local molecular chain formation micro orientation, according to the humidity in film lacing film drying process each stage, strict control drying temperature, make the non-rubber substance that rubber does not destroy rubber molecular chain as much as possible in drying process and shields to molecular chain, therefore, make product can keep resistance to ozone and high-performance.
Production technique of the present invention is simple, owing to combining natural air drying and hot blast combination drying process, production cost is low, links adopts and controls to destroy minimum technological process control to rubber molecular chain, control nitrogen content, remain resistance to ozone and the ageing-resistant protein having larger effect, reduce heat generation, lacing film is utilized to make molecular chain be subject to washing is broken, broken molecule chain is made again to recover after tearing, and form local molecular chain micro orientation, strictly drying temperature is controlled according to each step humidity of film lacing film drying process, make the non-rubber substance that rubber does not destroy rubber molecular chain as much as possible in drying process and shields to molecular chain, maintain resistance to ozone and the high-performance of product, good product quality, the production rate of recovery is high, production process environmental protection, production economy is efficient.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is described in further detail.Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.The experimental technique of unreceipted actual conditions in the following example, usually conveniently condition, or according to the condition that manufacturer advises.
Measure the chemical composition of rubber and performance, its testing method is as follows:
(1) chemical analysis of rubber
With the conventional instrument test total solids level of rubber, drc, nitrogen content, foreign matter content, ash oontent and acetone extract content etc.
(2) mensuration of properties
Respectively with mooney viscosity, the plasticity initial value P0 and antioxygen indices P RI of mooney viscosity instrument, vulkameter, tension testing machine, Wallace's plastometer, thermo-oxidative ageing case and ozone ageing case mensuration caouttchouc, the vulcanization characteristics of rubber unvulcanizate and the mechanical property of cross-linked rubber, thermogenesis performance, thermal-oxidative aging property and resistance to ozone cracking energy.
Embodiment one
Get that drc is 28%, ammonia content is that the fresh PRIM600 natural rubber latex 1000Kg of 0.008% is in mixing pit, adding proteolytic enzyme and standard compliant clear water regulates drc to 24%, adopt and determine that concentration is the formic acid consumption of 2% as calculated afterwards, warp also flows acid adding to coagulating pan, latex mixes 10 minutes and occurs flocculation, and slaking forms the grumeleuse without plain boiled water for 15 hours.Grumeleuse obtains resistance to ozone high-property natural rubber product after ironed dehydration, washing, compressing tablet (wherein: film stock thickness 7 ~ 9mm, nitrogen content 0.20%), lacing film (temperature 60 C) granulation in dry 5 days, drying, measures quality index and the performance of dry glue.
Quality index and performance: foreign matter content is 0.015%, plasticity initial value P0 is 50, and plasticity retention(percentage) PRI is 90%, and the ash content of coal is 0.2%, nitrogen content 0.20%, Mooney viscosity 82 unit; The curing time T-90 of pure glue formula is 8 minutes, and tensile strength is 27.5MPa, and elongation rate of tensile failure is 900%, and heat generation is 13 DEG C, heatproof air aging performance conservation rate 88%, and the resistance to ozone-induced cracking time is 8.5 hours.
Embodiment two
Get that drc is 32%, ammonia content is that the fresh PR107 natural rubber latex 1000Kg of 0.006% is in mixing pit, adding proteolytic enzyme and standard compliant clear water regulates drc to 24%, adopt and determine that concentration is the formic acid consumption of 2% as calculated afterwards, warp also flows acid adding to coagulating pan, latex mixes 8 minutes and occurs flocculation, and slaking forms the grumeleuse without plain boiled water for 15 hours.Grumeleuse obtains high-property natural rubber product after ironed dehydration, washing, compressing tablet (wherein: film stock thickness 8 ~ 9mm, nitrogen content 0.25%), lacing film (temperature 55 DEG C), granulation in dry 6 days, drying, measures quality index and the performance of dry glue.
Quality index and performance: foreign matter content is 0.015%, plasticity initial value P0 is 50, and plasticity retention(percentage) PRI is 90%, nitrogen content 0.25%, and the ash content of coal is 0.18%, Mooney viscosity 82 unit; The curing time T-90 of pure glue formula is 7 minutes, and tensile strength is 27.0MPa, and elongation rate of tensile failure is 880%, and heat generation is 16 DEG C, heatproof air aging performance conservation rate 88%, and the resistance to ozone-induced cracking time is 7.5 hours.
Embodiment three
Get the fresh heat that drc is 30%, ammonia content is 0.005% and grind 7-33-97 natural rubber latex 1000Kg in mixing pit, adding proteolytic enzyme and standard compliant clear water regulates drc to 22%, adopt and determine that concentration is the formic acid consumption of 2% as calculated afterwards, warp also flows acid adding to coagulating pan, latex mixes 8 minutes and occurs flocculation, and slaking forms the grumeleuse without plain boiled water for 15 hours.Grumeleuse obtains high-property natural rubber product after ironed dehydration, washing, granulation, compressing tablet (wherein: film stock thickness 7 ~ 9mm, nitrogen content 0.18%), lacing film (temperature 65 DEG C), granulation in dry 9 days, drying, measures quality index and the performance of dry glue.
Quality index and performance: foreign matter content is 0.013%, plasticity initial value P0 is 50, and plasticity retention(percentage) PRI is 92%, nitrogen content 0.18%, and the ash content of coal is 0.16%, Mooney viscosity 80 unit; The curing time T-90 of pure glue formula is 10 minutes, and tensile strength is 27.7MPa, and elongation rate of tensile failure is 900%, and heat generation is 15 DEG C, heatproof air aging performance conservation rate 91%, and the resistance to ozone-induced cracking time is 8 hours.
Embodiment four
Get drc be 73% heat grind the rubber pig of the natural coagulation of 72059 strains, through fully immersion, stripping and slicing, grumeleuse, after ironed dehydration, washing, compressing tablet (wherein: film stock thickness 9 ~ 10mm, nitrogen content 0.25%), lacing film (temperature 50 C), granulation in dry 6 days, drying, measures quality index and the performance of dry glue.
Quality index and performance: foreign matter content is 0.018%, plasticity initial value P0 is 50, and plasticity retention(percentage) PRI is 90%, nitrogen content 0.25%, and the ash content of coal is 0.25%, Mooney viscosity 80 unit; The curing time T-90 of pure glue formula is 7 minutes, and tensile strength is 26.5MPa, and elongation rate of tensile failure is 850%, and heat generation is 19 DEG C, heatproof air aging performance conservation rate 88%, and the resistance to ozone-induced cracking time is 6.0 hours.
Embodiment five
Get the fresh heat that drc is 28%, ammonia content is 0.005% and grind 87-9 natural rubber latex 1000Kg in mixing pit, adding standard compliant clear water regulates drc to 24%, add aqueous solution of protease, warp also flows enzyme-added to coagulating pan, latex mixes 60 minutes and occurs flocculation, and slaking forms the grumeleuse without plain boiled water for 16 hours.Grumeleuse obtains high-property natural rubber product after ironed dehydration, washing, compressing tablet (wherein: film stock thickness 7 ~ 9mm, nitrogen content 0.18%), lacing film (temperature 75 DEG C), granulation in dry 8 days, drying, measures quality index and the performance of dry glue.
Quality index and performance: foreign matter content is 0.016%, plasticity initial value P0 is 46, and plasticity retention(percentage) PRI is 92%, nitrogen content 0.18%, and the ash content of coal is 0.23%, Mooney viscosity 78 unit; The curing time T-90 of pure glue formula is 9 minutes, and tensile strength is 27.0MPa, and elongation rate of tensile failure is 900%, and heat generation is 18 DEG C, heatproof air aging performance conservation rate 90%, and the resistance to ozone-induced cracking time is 7 hours.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (3)
1. a production method for resistance to ozone high-property natural rubber, is characterized in that, its concrete steps are as follows:
1), get drc and be 8 ~ 62% and the fresh natural rubber latex of natural rubber strain that the associated proteins of interpolation less than 0.05% ammonia is suitable by weight percentage, adding Sumizyme MP adopts freezing method to solidify fresh latex and obtain flocculent gel, and its Control of Nitrogen Content is 0.15 ~ 0.35%; Flocculent gel being obtained grumeleuse or sheet rubber through solidifying with slaking, through ironed dehydration, washing, granulation, being pressed into the film that thickness is 2 ~ 15mm; Described associated proteins is suitable refers to that in fresh latex, rubber river flowing from Guizhou Province through Hunan into Dongting Lake albumen accounts for 10 ~ 40% of Tot Prot;
2), by film loft dried, control temperature is 15 ~ 120 DEG C, and the loft dried time is 1 ~ 15 day;
3), the film through loft dried is carried out granulation, drying can obtain resistance to ozone high-property natural rubber product.
2. production method according to claim 1, is characterized in that: the natural rubber strain that described associated proteins is suitable comprises PRIM600, heat grinds 7-33-97, heat grinds 879, heat grinds 72059 or PR107.
3. production method according to claim 1, is characterized in that: described Sumizyme MP refers to that enzyme activity is greater than 6KPPU/g in the basic conditions, and total plate count is less than 10000/G.
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Cited By (5)
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| CN107522913A (en) * | 2017-09-19 | 2017-12-29 | 润益康地（上海）物资贸易有限公司 | A kind of preparation method of Heveatex and the coprecipitated epoxy glue of white carbon liquid phase |
| CN108794658A (en) * | 2018-06-15 | 2018-11-13 | 海南省先进天然橡胶复合材料工程研究中心有限公司 | A method of preparing high performance heat resistant oxygen aging natural rubber |
| CN109181032A (en) * | 2018-09-21 | 2019-01-11 | 中国热带农业科学院农产品加工研究所 | A kind of ageing-resistant natural rubber raw rubber and preparation method thereof |
| CN109968558A (en) * | 2019-05-10 | 2019-07-05 | 勐腊田野橡胶销售有限责任公司 | A kind of rubber special production line |
| CN112592417A (en) * | 2020-12-09 | 2021-04-02 | 中国化工集团曙光橡胶工业研究设计院有限公司 | Aircraft tire natural rubber solidification system, application method thereof and aircraft tire natural rubber |
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| CN101519461A (en) * | 2009-03-25 | 2009-09-02 | 廖芸 | Method for solidifying nature rubber latex with microwave radiation |
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| CN107522913A (en) * | 2017-09-19 | 2017-12-29 | 润益康地（上海）物资贸易有限公司 | A kind of preparation method of Heveatex and the coprecipitated epoxy glue of white carbon liquid phase |
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| CN109181032A (en) * | 2018-09-21 | 2019-01-11 | 中国热带农业科学院农产品加工研究所 | A kind of ageing-resistant natural rubber raw rubber and preparation method thereof |
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| CN109968558A (en) * | 2019-05-10 | 2019-07-05 | 勐腊田野橡胶销售有限责任公司 | A kind of rubber special production line |
| CN112592417A (en) * | 2020-12-09 | 2021-04-02 | 中国化工集团曙光橡胶工业研究设计院有限公司 | Aircraft tire natural rubber solidification system, application method thereof and aircraft tire natural rubber |
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