CN103387677A - Preparation methods of lignin rubber additive and tyre rubber - Google Patents

Preparation methods of lignin rubber additive and tyre rubber Download PDF

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CN103387677A
CN103387677A CN2013103055798A CN201310305579A CN103387677A CN 103387677 A CN103387677 A CN 103387677A CN 2013103055798 A CN2013103055798 A CN 2013103055798A CN 201310305579 A CN201310305579 A CN 201310305579A CN 103387677 A CN103387677 A CN 103387677A
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rubber
xylogen
ingredients
lignin
mass ratio
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CN103387677B (en
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唐一林
江成真
焦峰
董岳
徐秋石
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Jinan Shengquan Group Share Holding Co Ltd
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Jinan Shengquan Group Share Holding Co Ltd
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Abstract

The invention provides preparation methods of a lignin rubber additive and tyre rubber. The preparation method of the lignin rubber additive comprises the following steps of mixing alkali lignin and an alkali liquor to obtain an alkali lignin solution, and filtering the alkali lignin solution by a nanofiltration membrane to obtain the lignin rubber additive, wherein the lignin rubber additive has weight-average molecular weight of 100-1000. The lignin rubber additive obtained by the preparation method can improve wear resistance of rubber and the preparation method has simple processes. Compared with the common tyre rubber, the tyre rubber with the lignin rubber additive has better wear resistance and has other performance indexes in a normal value scope.

Description

The preparation method of a kind of xylogen rubber ingredients and rubber for tire
Technical field
The invention belongs to the rubber ingredients technical field, relate in particular to the preparation method of a kind of xylogen rubber ingredients and rubber for tire.
Background technology
Rubber is from extracting plant or after synthetic, and reprocessing is made has the macromolecular material of elasticity, insulativity, waterproof and air, and elastomeric material is widely used in industry or life each side.But elastomeric material, without enhancing, often is difficult to obtain higher physical strength, adds the reinforcing rubber auxiliary agent can improve significantly the physical and mechanical properties of elastomeric material.
Reinforcing rubber auxiliary agent commonly used has the macromolecular materials such as the powder material such as carbon black, potter's clay and resin, xylogen.Along with the understanding of the problems such as mankind's environmental pollution and crisis of resource deepens continuously, the character such as that natural polymer has is renewable, degradable comes into one's own day by day, and therefore, xylogen is subject to people as the reinforcing rubber auxiliary agent and more and more pays close attention to.
Xylogen is the class material that the aromatic alcohol by polymerization forms, and is present in lignum, and Main Function is to carry out the sclereid wall by the formation net that interweaves, and mainly between cellulosic fibre, plays the resistance to compression effect.And contain many different active function groups such as conjugated double bond, aromatic base, phenolic hydroxyl group, alcoholic extract hydroxyl group, carbonyl, methoxyl group and carboxyl in lignin molecule, the advantage such as also have simultaneously renewable, degradable, nontoxic, reserves are large, therefore the application in Rubber Chemicals Industries is day by day extensive.But; because xylogen is a kind of amorphous thermoplastic polymers; second-order transition temperature higher with and the characteristic of the natural polymer that has, can affect the over-all properties of cross-linked rubber as rubber ingredients the time, therefore have limitation in the industrial scale application always.
In prior art, the application as rubber ingredients of multiple xylogen and modification derivant thereof is disclosed, xylogen after methylolation or methylolation again with the coprecipitated modification of synthetical glue after alternative carbon black make weighting agent, substitute that silicone resin is made linking agent and alternative reinforced resin is made strengthening agent etc.As disclosing the method for a kind of xylogen as rubber reinforcing filler in CN1044477A, at first it add formaldehyde and make the xylogen formaldehyde resin in concentrated papermaking wastewater, add in proportion again sulphur, zinc oxide, stearic acid, vulcanization accelerator, vulcanization activator, and with rubber, vulcanize at a certain temperature.But above-mentioned with xylogen as the method for strengthening agent, the wear resistance that its prepared rubber can not Reinforced Rubber, and preparation process is loaded down with trivial details.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of preparation method of xylogen rubber ingredients, and xylogen rubber ingredients provided by the invention can increase the fastness to rubbing of rubber, and preparation process is simple.
The invention discloses a kind of preparation method of xylogen rubber ingredients, comprise the following steps:
A) with alkali lignin with obtain alkali lignin solution after alkali lye mixes;
B) will obtain the xylogen rubber ingredients after the nanofiltration membrane filtration of above-mentioned alkali lignin solution with alkaline-resisting material; The weight-average molecular weight of described xylogen rubber ingredients is 100~1000.
Preferably, the mass ratio of described alkali lignin and alkali lye is (0.1~0.5): 1, and the mass concentration of described alkali lye is 0.5%~5%.
Preferably, described alkali lye is sodium hydroxide solution, potassium hydroxide solution, rubidium hydroxide solution or cesium hydroxide solution.
Preferably, described filtration time is 1~4 hour, and the temperature of described filtration is 50~80 ℃.
Preferably, described step B) be specially:
B1) will obtain the small molecules lignin liquor after the nanofiltration membrane filtration of alkali lignin solution with alkaline-resisting material;
B2) with the small molecules lignin liquor after acid out or spraying drying, obtain the xylogen rubber ingredients.
The invention discloses a kind of rubber for tire, it is characterized in that, comprise rubber, carbon black, rubber ingredients and xylogen rubber ingredients;
Described xylogen rubber ingredients prepare by the following method:
A) with alkali lignin with obtain alkali lignin solution after alkali lye mixes;
B) will obtain the xylogen rubber ingredients after the nanofiltration membrane filtration of above-mentioned alkali lignin solution with alkaline-resisting material; The weight-average molecular weight of described xylogen rubber ingredients is 100~1000;
The mass ratio of described rubber, carbon black and xylogen rubber ingredients is 100:(35~55): (1~5).
Preferably, described carbon black is carbon black N234.
Preferably, described rubber ingredients are rubber filling oil, rubber emulsifying agent, activating agent for rubber, rubber antioxidant, rubber accelerator and Cure of Rubber agent.
Preferably, described rubber filling oil is naphthenic oil; Described rubber emulsifying agent is stearic acid; Described activating agent for rubber is zinc oxide;
The mass ratio of described naphthenic oil and rubber is (1.5~2.5): 100; The mass ratio of described stearic acid and rubber is (2.5~3.5): 100; The mass ratio of described zinc oxide and rubber is (4.5~5.5): 100.
Preferably, described rubber antioxidant is Microcrystalline Wax, anti-aging agent RD and anti-aging agent 4030; Described rubber accelerator is accelerant CZ; Described Cure of Rubber agent is sulphur;
The mass ratio of described Microcrystalline Wax and rubber is (0.5~1.5): 100; The mass ratio of described anti-aging agent RD and rubber is (1.5~2.5): 100; Described anti-aging agent 4030 is (1.0~2.0) with the mass ratio of rubber: 100; The mass ratio of described accelerant CZ and rubber is (0.5~1.5): 100; The mass ratio of described sulphur and rubber is (0.5~1.5): 100.
The invention provides a kind of preparation method of xylogen rubber ingredients, with alkali lignin with obtain alkali lignin solution after alkali lye mixes, then to obtain weight-average molecular weight after above-mentioned alkali lignin solution is filtered with nanofiltration membrane be 100~1000 xylogen rubber ingredients.The present invention also provides a kind of rubber for tire, comprises the xylogen rubber ingredients that rubber, carbon black, rubber ingredients and above-mentioned preparation method obtain, and the mass ratio of rubber, carbon black and xylogen rubber ingredients is 100:(35~55): (1~5).Compared with prior art, xylogen rubber ingredients provided by the invention can increase the fastness to rubbing of rubber, and preparation process is simple; The rubber for tire of the above-mentioned xylogen rubber ingredients of use provided by the invention, fastness to rubbing increases to some extent than conventional tyre, and other performance index of rubber for tire are all in range of normal value.Experimental result shows, uses the rubber tyre of xylogen rubber ingredients preparation provided by the invention, and DIN abrasion volume has reduced 13%, Akron abrasion volume than the General Purpose Rubber tire and reduced 11%.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just in order to further illustrate the features and advantages of the present invention, rather than to the restriction of invention claim.
The invention provides a kind of preparation method of xylogen rubber ingredients, comprise the following steps:
A) with alkali lignin with obtain alkali lignin solution after alkali lye mixes;
B) after being filtered with the nanofiltration membrane with alkaline-resisting material, above-mentioned alkali lignin solution obtains the xylogen rubber ingredients; The weight-average molecular weight of described xylogen rubber ingredients is 100~1000.
The present invention with alkali lignin with obtain alkali lignin solution after alkali lye mixes, then to obtain weight-average molecular weight after above-mentioned alkali lignin solution is filtered with nanofiltration membrane be 100~1000 xylogen rubber ingredients.Xylogen rubber ingredients provided by the invention can increase the fastness to rubbing of rubber, and preparation process is simple.
All raw materials of the present invention, be not particularly limited its source, and that buys on market gets final product. 
The present invention at first with alkali lignin with obtain alkali lignin solution after alkali lye mixes, it is sodium hydroxide solution, potassium hydroxide solution, rubidium hydroxide solution or cesium hydroxide solution, more preferably sodium hydroxide solution and potassium hydroxide solution that described alkali lye is preferably alkali lye; The mass concentration of described alkali lye is preferably 0.5%~5%, and more preferably 1%~3%; The mass ratio of described alkali lignin and alkali lye is preferably (0.1~0.5): 1, more preferably (0.2~0.4): 1.The present invention is not particularly limited described mixing, is preferably and is dissolved in alkali lignin in alkali lye fully; The present invention is not particularly limited the condition of described mixing, with mixing condition well known to those skilled in the art, gets final product; The present invention is not particularly limited the device of described mixing, and mixing device well known to those skilled in the art gets final product; The present invention is not particularly limited the source of described alkali lignin, with commercially available alkali lignin, gets final product; The present invention is not particularly limited the purity of described alkali lignin, with conventional purity requirement well known to those skilled in the art, gets final product; The present invention is not particularly limited the molecular weight of described alkali lignin, with molecular weight conventional in commercially available alkali lignin, requires to get final product.
Then the present invention obtains the xylogen rubber ingredients after the above-mentioned alkali lignin solution that mixes is filtered with the nanofiltration membrane of alkaline-resisting material, and this process is preferably:
B1) will obtain the small molecules lignin liquor after the nanofiltration membrane filtration of alkali lignin solution with alkaline-resisting material;
B2) with the small molecules lignin liquor after acid out or spraying drying, obtain the xylogen rubber ingredients.
The present invention obtains the small molecules lignin liquor after at first alkali lignin being filtered with the nanofiltration membrane of alkaline-resisting material; The material of described nanofiltration membrane is preferably the nanofiltration membrane of alkaline-resisting material, more preferably the rolling nanofiltration membrane of alkaline-resisting material; Described small molecules xylogen weight-average molecular weight is preferably 100~1000, and more preferably 200~800; Described nanofiltration membrane molecular weight cut-off is preferably 100~1000, and more preferably 200~800; Described filtration time is preferably 1~4 hour, more preferably 2~3 hours; Described filtration temperature is preferably 50~80 ℃, more preferably 60~70 ℃; Described filtration is preferably circulating filtration; The present invention is not particularly limited the source of described nanofiltration membrane, buys and gets final product from the market; The present invention is not particularly limited other character of described nanofiltration membrane, with nanofiltration membrane well known to those skilled in the art, gets final product; The present invention is not particularly limited other conditions of described filtration, with filtration condition well known to those skilled in the art, gets final product.
Then the present invention after acid out, obtains the xylogen rubber ingredients with above-mentioned small molecules lignin liquor; Described acid out is preferably with sulfuric acid and carries out acid out, and sulfuric acid concentration is preferably 20%~50%, and more preferably 30%~40%; After described acid out, the pH value of small molecules lignin liquor is preferably 2~5, and more preferably 3~4.The present invention does not have other to be particularly limited to the method for described acid out, with acid out method well known to those skilled in the art, gets final product; The present invention is not particularly limited the equipment of described acid out, with acid out equipment well known to those skilled in the art, gets final product; The present invention is not particularly limited other conditions of described acid out, with acid out well known to those skilled in the art, requires to get final product.
The present invention preferably carries out the small molecules lignin liquor centrifugation, drying after acid out, obtain dry powdery xylogen.Described drying temperature is preferably 30~50 ℃, more preferably 35~45 ℃; Be preferably 6~10 hours described time of drying, more preferably 7~9 hours; The present invention is not particularly limited the condition of described centrifugation, with centrifugation condition well known to those skilled in the art, gets final product; The present invention is not particularly limited the equipment of described centrifugation, with centrifugal separation equipment well known to those skilled in the art, gets final product; The present invention is not particularly limited the equipment of described drying, with drying plant well known to those skilled in the art, gets final product.
The present invention is at above-mentioned steps B1) in obtain the small molecules lignin liquor after, also preferred by spraying drying, obtain dry powdery xylogen.The present invention is not particularly limited described spray-dired method, preferably adopts the pressure spray dryer method; The present invention is not particularly limited described spray-dired equipment, with spray drying device well known to those skilled in the art, gets final product; The present invention is not particularly limited described spray-dired condition, with spraying drying condition well known to those skilled in the art, gets final product.
The present invention preferably, to the washing of powdery xylogen process and the drying of the drying through the aforesaid method processing, removes residual acid and salinity, obtains finally highly purified xylogen rubber ingredients.Above-mentioned highly purified xylogen rubber ingredients second-order transition temperature is low, can scatter equably when compounding rubber.Described washing is preferably with glycerine or deionized water and washs, and more preferably with glycerine, washs; Described drying is preferably vacuum-drying; Described drying temperature is preferably 30~50 ℃, more preferably 35~45 ℃; Be preferably 1.5~4.5 hours described time of drying, more preferably 2~4 hours; The present invention is not particularly limited the method for washing, with washing methods well known to those skilled in the art, gets final product; The present invention is not particularly limited the equipment of washing, with washing plant well known to those skilled in the art, gets final product; The present invention is not particularly limited the equipment of drying, with drying plant well known to those skilled in the art, gets final product.
The present invention also provides a kind of rubber for tire, comprises rubber, carbon black, rubber ingredients and xylogen rubber ingredients; Described xylogen rubber ingredients prepare by the following method:
With alkali lignin with obtain alkali lignin solution after alkali lye mixes, then obtain the xylogen rubber ingredients after above-mentioned alkali lignin solution is filtered with nanofiltration membrane; The weight-average molecular weight of described xylogen rubber ingredients is 100~1000; The mass ratio of described rubber, carbon black and xylogen rubber ingredients is 100:(35~55): (1~5).
Rubber for tire provided by the present invention, comprise rubber, carbon black, rubber ingredients and xylogen rubber ingredients, and the mass ratio of rubber, carbon black and xylogen rubber ingredients is 100:(35~55): (1~5).The rubber for tire of the above-mentioned xylogen rubber ingredients of use provided by the invention, fastness to rubbing increases to some extent than conventional tyre, and other performance index of rubber for tire are all in range of normal value.
The present invention uses and comprises that rubber, carbon black, rubber ingredients and xylogen rubber ingredients prepare rubber for tire.The mass ratio of described rubber, carbon black and xylogen rubber ingredients is preferably 100:(35~55): (1~5), more preferably 100:(40~50): (2~3); Described carbon black is preferably carbon black N234; The present invention uses carbon black N234 as rubber reinforcing filler, and the mass ratio of described carbon black N234 and rubber is preferably (35~55): 100, more preferably (40~50): 100.
Rubber ingredients of the present invention are preferably rubber filling oil, rubber emulsifying agent, activating agent for rubber, rubber antioxidant, rubber accelerator and Cure of Rubber agent.Described rubber filling oil is preferably naphthenic oil, and the mass ratio of described naphthenic oil and rubber is preferably (1.5~2.5): 100, and 2.0:100 more preferably; Described rubber emulsifying agent is preferably stearic acid, and the mass ratio of described stearic acid and rubber is preferably (2.5~3.5): 100, and 3.0:100 more preferably; Described rubber activator is preferably zinc oxide, and the mass ratio of described zinc oxide and rubber is preferably (4.5~5.5): 100, and 5.0:100 more preferably; Described rubber antioxidant is preferably Microcrystalline Wax, anti-aging agent RD and antioxidant 4020, the mass ratio of described Microcrystalline Wax and rubber is preferably (0.5~1.5): 100,1.0:100 more preferably, the mass ratio of described anti-aging agent RD and rubber is preferably (1.5~2.5): 100,2.0:100 more preferably, the mass ratio of described antioxidant 4020 and rubber is preferably (1.0~2.0): 100, and 1.5:100 more preferably; Described rubber accelerator is preferably accelerant CZ, and the mass ratio of described accelerant CZ and rubber is preferably (0.5~1.5): 100, and 1.0:100 more preferably; Described Cure of Rubber agent is preferably sulphur, and the mass ratio of described sulphur and rubber is preferably (0.5~1.5): 100, and 1.0:100 more preferably.
In rubber for tire provided by the invention, the mass ratio of described xylogen rubber ingredients and rubber is preferably (1~5): 100, more preferably (2~4): 100; The preparation method of described xylogen rubber ingredients is identical with the preparation method of a kind of xylogen rubber ingredients disclosed by the invention, and the character of resulting xylogen rubber ingredients is also identical, therefore repeats no longer one by one.The present invention is not particularly limited the production technique of rubber for tire, with the production technique of rubber for tire well known to those skilled in the art, gets final product; The present invention is not particularly limited the processing parameter of rubber for tire, and the processing parameter of knowing rubber for tire with those skilled in the art gets final product.
The rubber for tire that uses the present invention to obtain the preparation of xylogen rubber ingredients is tested, result shows, use the rubber tyre of xylogen rubber ingredients preparation provided by the invention, DIN abrasion volume has reduced 13% than the General Purpose Rubber tire, Akron abrasion volume has reduced 11%, and other performance index of rubber for tire are all in range of normal value.
In order further to understand the present invention, below in conjunction with embodiment, the preparation method of a kind of xylogen rubber ingredients provided by the invention is described, protection scope of the present invention is not limited by the following examples.
Embodiment 1
The mass concentration of 50g NaOH being mixed system with 2500g water is 2% alkaline solution, the undressed commercially available alkali lignin of 500g (Shandong spring woods chemical industry company limited) being put into alkaline solution again and be stirred to fully to dissolve and obtain alkali lignin solution, is then 1000 rolling nanofiltration membrane circulating filtration with molecular weight cut-off with above-mentioned solution.After 2 hours, stop filtering and obtain the small molecules lignin liquor, and be heated to 70 ℃, then to slowly adding mass concentration in above-mentioned small molecules lignin liquor, be that 30% sulfuric acid carries out acid out, until filtrate pH value is 3.5.After acid out was complete, the small molecules xylogen mixed solution that above-mentioned acid out is obtained carried out centrifugation, obtains solid lignin, then solid lignin is placed in the baking oven inner drying, and drying temperature is 40 ℃, and be 8 hours time of drying, obtained dry powdery xylogen.
The powdery xylogen of above-mentioned drying is washed with glycerine, glycerine is filtered, the powdery xylogen after filtering is dry in vacuum drying oven, and drying temperature is 40 ℃ again, be 3 hours time of drying, obtains finally the 16g weight-average molecular weight less than 1000 xylogen rubber ingredients.
Embodiment 2
With the xylogen rubber ingredients of preparation in rubber, carbon black, rubber ingredients and embodiment 1, carry out mixing and sulfuration according to following formula, fill a prescription as follows:
Rubber 100g; Carbon black N234 45g; Naphthenic oil 2.0g; Stearic acid 3.0g; Zinc oxide 5.0g; Witcodur 272 1.0g; Anti-aging agent RD 2.0g; Antioxidant 4020 1.5g; Accelerant CZ 1.0g; Sulfur 1.0g; The xylogen rubber ingredients 2.0g of this patent preparation.
Carry out mixingly on the Banbury mixer of 1L, calendering process is as follows:
Table 1 rubber mixing-milling technique
Figure BDA00003539261200071
Figure BDA00003539261200081
Obtain the described rubber for tire A of this patent after above-mentioned technique is mixing 1
Embodiment 3
With the xylogen rubber ingredients of preparation in rubber, carbon black, rubber ingredients and embodiment 1, carry out mixing and sulfuration according to following formula, fill a prescription as follows:
Rubber 100g; Carbon black N234 45g; Naphthenic oil 2.0g; Stearic acid 3.0g; Zinc oxide 5.0g; Witcodur 272 1.0g; Anti-aging agent RD 2.0g; Antioxidant 4020 1.5g; Accelerant CZ 1.0g; Sulfur 1.0g; The xylogen rubber ingredients 1.0g of this patent preparation.
Carry out mixingly on the Banbury mixer of 1L, calendering process is as follows:
Table 2 rubber mixing-milling technique
Figure BDA00003539261200082
Figure BDA00003539261200091
Obtain the described rubber for tire A of this patent after above-mentioned technique is mixing 2
Embodiment 4
With the xylogen rubber ingredients of preparation in rubber, carbon black, rubber ingredients and embodiment 1, carry out mixing and sulfuration according to following formula, fill a prescription as follows:
Rubber 100g; Carbon black N234 45g; Naphthenic oil 2.0g; Stearic acid 3.0g; Zinc oxide 5.0g; Witcodur 272 1.0g; Anti-aging agent RD 2.0g; Antioxidant 4020 1.5g; Accelerant CZ 1.0g; Sulfur 1.0g; The xylogen rubber ingredients 5.0g of this patent preparation.
Carry out mixingly on the Banbury mixer of 1L, calendering process is as follows:
Table 3 rubber mixing-milling technique
Figure BDA00003539261200092
Obtain the described rubber for tire A of this patent after above-mentioned technique is mixing 3
Comparative example 1
With rubber, carbon black, rubber ingredients and undressed commercially available alkali lignin (Shandong spring woods chemical industry company limited), carry out mixing and sulfuration according to following formula, fill a prescription as follows:
Rubber 100g; Carbon black N234 45g; Naphthenic oil 2.0g; Stearic acid 3.0g; Zinc oxide 5.0g; Witcodur 272 1.0g; Anti-aging agent RD 2.0g; Antioxidant 4020 1.5g; Accelerant CZ 1.0g; Sulfur 1.0g; Untreated alkali lignin 2.0g.
Carry out mixingly on the Banbury mixer of 1L, calendering process is as follows:
Table 4 rubber mixing-milling technique
Obtain rubber for tire B after above-mentioned technique is mixing.
Comparative example 2
With rubber, carbon black, rubber ingredients and commercially available calcium lignin sulphonate (Gaotang, Shandong polynary xylogen company limited), carry out mixing and sulfuration according to following formula, fill a prescription as follows:
Rubber 100g; Carbon black N234 45g; Naphthenic oil 2.0g; Stearic acid 3.0g; Zinc oxide 5.0g; Witcodur 272 1.0g; Anti-aging agent RD 2.0g; Antioxidant 4020 1.5g; Accelerant CZ 1.0g; Sulfur 1.0g; Calcium lignin sulphonate 2.0g.
Carry out mixingly on the Banbury mixer of 1L, calendering process is as follows:
Table 5 rubber mixing-milling technique
Obtain rubber for tire C after above-mentioned technique is mixing.
Comparative example 3
With rubber, carbon black, rubber ingredients, carry out mixing and sulfuration according to following formula, fill a prescription as follows:
Rubber 100g; Carbon black N234 45g; Naphthenic oil 2.0g; Stearic acid 3.0g; Zinc oxide 5.0g; Witcodur 272 1.0g; Anti-aging agent RD 2.0g; Antioxidant 4020 1.5g; Accelerant CZ 1.0g; Sulfur 1.0g.
Carry out mixingly on the Banbury mixer of 1L, calendering process is as follows:
Table 6 rubber mixing-milling technique
Figure BDA00003539261200121
Obtain rubber for tire D after above-mentioned technique is mixing.
Embodiment 5
Rubber for tire A with preparation in embodiment 2,3 and 4 1, A 2And A 3Carry out the performance comparison experiment with rubber for tire B, C and the D of comparative example 1~3 preparation, comparing result is as follows:
Table 7 finished composition mooney viscosity table
Figure BDA00003539261200122
Figure BDA00003539261200123
Table 8 finished composition mooney scorch table (125 ℃)
Figure BDA00003539261200131
Table 9 finished composition curability table (150 ℃)
Figure BDA00003539261200132
Table 10 cross-linked rubber is torn and the tensile property table
Figure BDA00003539261200141
Table 11 cross-linked rubber hardness performance table
Table 12 cross-linked rubber rebound performance table
Figure BDA00003539261200143
Table 13 compression heat generation data sheet
Figure BDA00003539261200144
Figure BDA00003539261200151
Table 14DIN and Akron abrasion volume data table
Figure BDA00003539261200152
Above preparation method to a kind of xylogen rubber ingredients provided by the present invention and a kind of rubber for tire are described in detail.Applied a concrete example herein principle of the present invention and embodiment are set forth, the explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of the claims in the present invention.

Claims (10)

1. the preparation method of xylogen rubber ingredients comprises the following steps:
A) with alkali lignin with obtain alkali lignin solution after alkali lye mixes;
B) will obtain the xylogen rubber ingredients after the nanofiltration membrane filtration of above-mentioned alkali lignin solution with alkaline-resisting material;
The weight-average molecular weight of described xylogen rubber ingredients is 100~1000.
2. preparation method according to claim 1, is characterized in that, the mass ratio of described alkali lignin and alkali lye is (0.1~0.5): 1, and the mass concentration of described alkali lye is 0.5%~5%.
3. preparation method according to claim 1, is characterized in that, described alkali lye is sodium hydroxide solution, potassium hydroxide solution, rubidium hydroxide solution or cesium hydroxide solution.
4. preparation method according to claim 1, is characterized in that, the time of described filtration is 1~4 hour, and the temperature of filtration is 50~80 ℃.
5. preparation method according to claim 1, is characterized in that, described step B) be specially:
B1) will obtain the small molecules lignin liquor after the nanofiltration membrane filtration of alkali lignin solution with alkaline-resisting material;
B2) with the small molecules lignin liquor after acid out or spraying drying, obtain the xylogen rubber ingredients.
6. a rubber for tire, is characterized in that, comprises rubber, carbon black, rubber ingredients and xylogen rubber ingredients;
Described xylogen rubber ingredients prepare by the following method:
A) with alkali lignin with obtain alkali lignin solution after alkali lye mixes;
B) will obtain the xylogen rubber ingredients after the nanofiltration membrane filtration of above-mentioned alkali lignin solution with alkaline-resisting material; The weight-average molecular weight of described xylogen rubber ingredients is 100~1000;
The mass ratio of described rubber, carbon black and xylogen rubber ingredients is 100:(35~55): (1~5).
7. rubber for tire according to claim 6, is characterized in that, described carbon black is carbon black N234.
8. rubber for tire according to claim 6, is characterized in that, described rubber ingredients are rubber filling oil, rubber emulsifying agent, activating agent for rubber, rubber antioxidant, rubber accelerator and Cure of Rubber agent.
9. rubber for tire according to claim 6, is characterized in that, described rubber filling oil is naphthenic oil; Described rubber emulsifying agent is stearic acid; Described activating agent for rubber is zinc oxide;
The mass ratio of described naphthenic oil and rubber is (1.5~2.5): 100; The mass ratio of described stearic acid and rubber is (2.5~3.5): 100; The mass ratio of described zinc oxide and rubber is (4.5~5.5): 100.
10. rubber for tire according to claim 6, is characterized in that, described rubber antioxidant is Microcrystalline Wax, anti-aging agent RD and anti-aging agent 4030; Described rubber accelerator is accelerant CZ; Described Cure of Rubber agent is sulphur;
The mass ratio of described Microcrystalline Wax and rubber is (0.5~1.5): 100; The mass ratio of described anti-aging agent RD and rubber is (1.5~2.5): 100; Described anti-aging agent 4030 is (1.0~2.0) with the mass ratio of rubber: 100; The mass ratio of described accelerant CZ and rubber is (0.5~1.5): 100; The mass ratio of described sulphur and rubber is (0.5~1.5): 100.
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Cited By (8)

* Cited by examiner, † Cited by third party
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CN113185755A (en) * 2021-04-14 2021-07-30 杭州中策橡胶循环科技有限公司 Cushion rubber for retreading tire and production process thereof

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CN103756060A (en) * 2013-12-16 2014-04-30 华南理工大学 Rubber composite material filled by cardanol modified lignin and preparation method thereof
CN105960433A (en) * 2014-02-03 2016-09-21 株式会社普利司通 Rubber compounds containing silicon dioxide for the production of tyres
CN105960433B (en) * 2014-02-03 2018-03-30 株式会社普利司通 Tire production wraps silica containing Rubber compound
CN107531954A (en) * 2015-04-24 2018-01-02 花王株式会社 Resin additive
US10717852B2 (en) 2015-04-24 2020-07-21 Kao Corporation Additive for resins
CN107446219A (en) * 2017-09-25 2017-12-08 安徽依采妮纤维材料科技有限公司 A kind of preparation method of lignin plastic composite
CN107722396A (en) * 2017-10-16 2018-02-23 华南理工大学 A kind of lignin/carbon black/nitile-butadiene rubber composite material and preparation method thereof
CN107722396B (en) * 2017-10-16 2020-06-19 华南理工大学 Lignin/carbon black/nitrile rubber composite material and preparation method thereof
CN109111749A (en) * 2018-07-13 2019-01-01 安徽省含山县锦华氧化锌厂 A kind of modified rubber auxiliary agent containing lignin
CN110724317A (en) * 2018-07-16 2020-01-24 中国石油化工股份有限公司 Environment-friendly tire side rubber material
CN110724317B (en) * 2018-07-16 2022-08-12 中国石油化工股份有限公司 Environment-friendly tire side rubber material
CN113185755A (en) * 2021-04-14 2021-07-30 杭州中策橡胶循环科技有限公司 Cushion rubber for retreading tire and production process thereof

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