CN103387677B - The preparation method of a kind of xylogen rubber ingredients and rubber for tire - Google Patents
The preparation method of a kind of xylogen rubber ingredients and rubber for tire Download PDFInfo
- Publication number
- CN103387677B CN103387677B CN201310305579.8A CN201310305579A CN103387677B CN 103387677 B CN103387677 B CN 103387677B CN 201310305579 A CN201310305579 A CN 201310305579A CN 103387677 B CN103387677 B CN 103387677B
- Authority
- CN
- China
- Prior art keywords
- rubber
- xylogen
- ingredients
- mass ratio
- alkali
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides the preparation method of a kind of xylogen rubber ingredients and rubber for tire, comprise the following steps: after being mixed with alkali lye by alkali lignin, obtain alkali lignin solution, obtain xylogen rubber ingredients by after above-mentioned alkali lignin solution nanofiltration membrane again, the weight-average molecular weight of described xylogen rubber ingredients is 100 ~ 1000.The xylogen rubber ingredients that preparation method provided by the invention obtains can increase the fastness to rubbing of rubber, and preparation process is simple.The rubber for tire of the xylogen rubber ingredients using the present invention to prepare, fastness to rubbing comparatively conventional tyre increases to some extent, and other performance index of rubber for tire are all in range of normal value.
Description
Technical field
The invention belongs to rubber ingredients technical field, particularly relate to the preparation method of a kind of xylogen rubber ingredients and rubber for tire.
Background technology
Rubber to extract from plant or after synthetic, and the macromolecular material of what reprocessing was made have elasticity, insulativity, waterproof and air, elastomeric material is widely used in industry or life each side.But elastomeric material is without enhancing, be often difficult to obtain higher physical strength, add the physical and mechanical properties that reinforcing rubber auxiliary agent can improve elastomeric material significantly.
Conventional reinforcing rubber auxiliary agent has the powder material such as carbon black, potter's clay and the macromolecular material such as 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 renewable, degradable that natural polymer has comes into one's own day by day, and therefore, xylogen is subject to people as reinforcing rubber auxiliary agent and more and more pays close attention to.
Xylogen is the class material be made up of the aromatic alcohol be polymerized, and is present in lignum, and Main Function carrys out sclereid wall by forming intertexture net, mainly between cellulosic fibre, plays resistance to compression effect.And containing many different active function groups such as conjugated double bond, aromatic base, phenolic hydroxyl group, alcoholic extract hydroxyl group, carbonyl, methoxyl group and carboxyls in lignin molecule, also there is renewable, degradable simultaneously, the advantage such as nontoxic, reserves are large, the application therefore in Rubber Chemicals Industries is day by day extensive.But; because xylogen is a kind of amorphous thermoplastic polymers;, as the over-all properties that can affect cross-linked rubber during rubber ingredients, therefore in industrial scale application, there is limitation in the characteristic of higher and its natural polymer had of second-order transition temperature always.
In prior art, disclose the application as rubber ingredients of multiple xylogen and modification derivant thereof, xylogen after methylolation or methylolation again with synthetical glue coprecipitated modified alternative carbon black make weighting agent, substitute silicone resin and make linking agent and alternative reinforced resin makes strengthening agent etc.As disclosed the method for a kind of xylogen as rubber reinforcing filler in CN1044477A, first it add formaldehyde and make xylogen formaldehyde resin in concentrated papermaking wastewater, add sulphur, zinc oxide, stearic acid, vulcanization accelerator, vulcanization activator in proportion again, and carry out sulfuration at a certain temperature with rubber.But above-mentioned xylogen is as the method for strengthening agent, the rubber prepared by it can not the wear resistance of 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 the preparation method providing a kind 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) alkali lignin solution is obtained after being mixed with alkali lye by alkali lignin;
B) xylogen rubber ingredients are obtained by after the nanofiltration membrane of above-mentioned alkali lignin solution by 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 DEG C.
Preferably, described step B) be specially:
B1) small molecules lignin liquor is obtained by after the nanofiltration membrane of alkali lignin solution by alkaline-resisting material;
B2) by small molecules lignin liquor after acid out or spraying dry, obtain 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 are prepared by the following method:
A) alkali lignin solution is obtained after being mixed with alkali lye by alkali lignin;
B) xylogen rubber ingredients are obtained by after the nanofiltration membrane of above-mentioned alkali lignin solution by 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, latex rubber agent, activating agent for rubber, rubber antioxidant, rubber accelerator and Cure of Rubber agent.
Preferably, described rubber filling oil is naphthenic oil; Described latex rubber 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, after being mixed with alkali lye by alkali lignin, obtain alkali lignin solution, then the xylogen rubber ingredients that weight-average molecular weight is 100 ~ 1000 will be obtained after above-mentioned alkali lignin solution nanofiltration membrane.Present invention also offers a kind of rubber for tire, comprise the xylogen rubber ingredients that rubber, carbon black, rubber ingredients and above-mentioned preparation method obtain, 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 comparatively conventional tyre increases to some extent, and other performance index of rubber for tire are all in range of normal value.Experimental result shows, uses rubber tyre prepared by xylogen rubber ingredients provided by the invention, and DIN wear volume comparatively General Purpose Rubber tire decreases 13%, Akron wear volume and decreases 11%.
Embodiment
In order to understand the present invention further, 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, instead of the restriction to invention claim.
The invention provides a kind of preparation method of xylogen rubber ingredients, comprise the following steps:
A) alkali lignin solution is obtained after being mixed with alkali lye by alkali lignin;
B) above-mentioned alkali lignin solution is obtained xylogen rubber ingredients with after the nanofiltration membrane by alkaline-resisting material; The weight-average molecular weight of described xylogen rubber ingredients is 100 ~ 1000.
The present invention obtains alkali lignin solution after being mixed with alkali lye by alkali lignin, then will obtain the xylogen rubber ingredients that weight-average molecular weight is 100 ~ 1000 after above-mentioned alkali lignin solution nanofiltration membrane.Xylogen rubber ingredients provided by the invention can increase the fastness to rubbing of rubber, and preparation process is simple.
The all raw materials of the present invention, are not particularly limited its source, commercially buy.
The present invention obtains alkali lignin solution after first being mixed with alkali lye by alkali lignin, it is sodium hydroxide solution, potassium hydroxide solution, rubidium hydroxide solution or cesium hydroxide solution that described alkali lye is preferably alkali lye, is more preferably sodium hydroxide solution and potassium hydroxide solution; The mass concentration of described alkali lye is preferably 0.5% ~ 5%, is more preferably 1% ~ 3%; The mass ratio of described alkali lignin and alkali lye is preferably (0.1 ~ 0.5): 1, is more preferably (0.2 ~ 0.4): 1.The present invention is not particularly limited described mixing, is preferably dissolved in completely in alkali lye by alkali lignin; The condition of the present invention to described mixing is not particularly limited, with mixing condition well known to those skilled in the art; The device of the present invention to described mixing is not particularly limited, mixing device well known to those skilled in the art; The source of the present invention to described alkali lignin is not particularly limited, with commercially available alkali lignin; The purity of the present invention to described alkali lignin is not particularly limited, with conventional purity requirement well known to those skilled in the art; The molecular weight of the present invention to described alkali lignin is not particularly limited, with molecular weight requirement conventional in commercially available alkali lignin.
Then the above-mentioned alkali lignin solution mixed is obtained xylogen rubber ingredients with after the nanofiltration membrane of alkaline-resisting material by the present invention, and this process is preferably:
B1) small molecules lignin liquor is obtained by after the nanofiltration membrane of alkali lignin solution by alkaline-resisting material;
B2) by small molecules lignin liquor after acid out or spraying dry, obtain xylogen rubber ingredients.
First the present invention obtains small molecules lignin liquor by after the nanofiltration membrane of alkali lignin by alkaline-resisting material; The material of described nanofiltration membrane is preferably the nanofiltration membrane of alkaline-resisting material, is more preferably the rolling nanofiltration membrane of alkaline-resisting material; Described small molecules xylogen weight-average molecular weight is preferably 100 ~ 1000, is more preferably 200 ~ 800; Described nanofiltration membrane molecular weight cut-off is preferably 100 ~ 1000, is more preferably 200 ~ 800; Described filtration time is preferably 1 ~ 4 hour, is more preferably 2 ~ 3 hours; Described filtration temperature is preferably 50 ~ 80 DEG C, is more preferably 60 ~ 70 DEG C; Described filtration is preferably circulating filtration; The source of the present invention to described nanofiltration membrane is not particularly limited, commercially; The present invention's other character to described nanofiltration membrane are not particularly limited, with nanofiltration membrane well known to those skilled in the art; The present invention's other conditions to described filtration are not particularly limited, with filtration condition well known to those skilled in the art.
Then the present invention is by above-mentioned small molecules lignin liquor after acid out, obtains xylogen rubber ingredients; Described acid out preferably carries out acid out with sulfuric acid, and sulfuric acid concentration is preferably 20% ~ 50%, is more preferably 30% ~ 40%; After described acid out, the pH value of small molecules lignin liquor is preferably 2 ~ 5, is more preferably 3 ~ 4.The method of the present invention to described acid out does not have other to be particularly limited to, with acid out method well known to those skilled in the art; The equipment of the present invention to described acid out is not particularly limited, with acid out equipment well known to those skilled in the art; The present invention's other conditions to described acid out are not particularly limited, and require with acid out well known to those skilled in the art.
Small molecules lignin liquor is preferably carried out centrifugation, drying by the present invention after acid out, obtains dry powdery xylogen.Described drying temperature is preferably 30 ~ 50 DEG C, is more preferably 35 ~ 45 DEG C; Described time of drying is preferably 6 ~ 10 hours, is more preferably 7 ~ 9 hours; The condition of the present invention to described centrifugation is not particularly limited, with centrifugation condition well known to those skilled in the art; The equipment of the present invention to described centrifugation is not particularly limited, with centrifugal separation equipment well known to those skilled in the art; The equipment of the present invention to described drying is not particularly limited, with drying plant well known to those skilled in the art.
The present invention is at above-mentioned steps B1) in obtain small molecules lignin liquor after, also preferably by spraying dry, obtain dry powdery xylogen.The present invention is not particularly limited described spray-dired method, preferably adopts 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; The present invention is not particularly limited described spray-dired condition, with spray drying condition well known to those skilled in the art.
The present invention preferably passes through washing and drying to the powdery xylogen of the drying through aforesaid method process, removes residual acid and salinity, finally obtains 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 washed with glycerine or deionized water, is more preferably and washs with glycerine; Described drying is preferably vacuum-drying; Described drying temperature is preferably 30 ~ 50 DEG C, is more preferably 35 ~ 45 DEG C; Described time of drying is preferably 1.5 ~ 4.5 hours, is more preferably 2 ~ 4 hours; The method of the present invention to washing is not particularly limited, with washing methods well known to those skilled in the art; The equipment of the present invention to washing is not particularly limited, with washing plant well known to those skilled in the art; The equipment of the present invention to drying is not particularly limited, with drying plant well known to those skilled in the art.
Present invention also offers a kind of rubber for tire, comprise rubber, carbon black, rubber ingredients and xylogen rubber ingredients; Described xylogen rubber ingredients are prepared by the following method:
Obtain alkali lignin solution after being mixed with alkali lye by alkali lignin, then obtain xylogen rubber ingredients by after above-mentioned alkali lignin solution 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, comprises 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 comparatively conventional tyre increases to some extent, and other performance index of rubber for tire are all in range of normal value.
The present invention's use comprises rubber, carbon black, rubber ingredients and xylogen rubber ingredients and prepares rubber for tire.The mass ratio of described rubber, carbon black and xylogen rubber ingredients is preferably 100:(35 ~ 55): (1 ~ 5), is 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, is more preferably (40 ~ 50): 100.
Rubber ingredients of the present invention are preferably rubber filling oil, latex rubber 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, is more preferably 2.0:100; Described latex rubber agent is preferably stearic acid, and the mass ratio of described stearic acid and rubber is preferably (2.5 ~ 3.5): 100, is more preferably 3.0:100; Described rubber activator is preferably zinc oxide, and the mass ratio of described zinc oxide and rubber is preferably (4.5 ~ 5.5): 100, is more preferably 5.0:100; 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, be more preferably 1.0:100, the mass ratio of described anti-aging agent RD and rubber is preferably (1.5 ~ 2.5): 100, be more preferably 2.0:100, the mass ratio of described antioxidant 4020 and rubber is preferably (1.0 ~ 2.0): 100, is more preferably 1.5:100; Described rubber accelerator is preferably accelerant CZ, and the mass ratio of described accelerant CZ and rubber is preferably (0.5 ~ 1.5): 100, is more preferably 1.0:100; Described Cure of Rubber agent is preferably sulphur, and the mass ratio of described sulphur and rubber is preferably (0.5 ~ 1.5): 100, is more preferably 1.0:100.
In rubber for tire provided by the invention, the mass ratio of described xylogen rubber ingredients and rubber is preferably (1 ~ 5): 100, is 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 the xylogen rubber ingredients obtained is also identical, therefore repeats no longer one by one.The production technique of the present invention to rubber for tire is not particularly limited, with the production technique of rubber for tire well known to those skilled in the art; The processing parameter of the present invention to rubber for tire is not particularly limited, and knows the processing parameter of rubber for tire with those skilled in the art.
Obtain rubber for tire prepared by xylogen rubber ingredients to using the present invention to test, result shows, use rubber tyre prepared by xylogen rubber ingredients provided by the invention, DIN wear volume comparatively General Purpose Rubber tire decreases 13%, Akron wear volume decreases 11%, and other performance index of rubber for tire are all in range of normal value.
In order to understand the present invention further, below in conjunction with embodiment, the preparation method to a kind of xylogen rubber ingredients provided by the invention is described, and protection scope of the present invention is not limited by the following examples.
Embodiment 1
The mass concentration mixing of 50gNaOH and 2500g water made is the alkaline solution of 2%, again undressed for 500g commercially available alkali lignin (Shandong Quan Lin Chemical Co., Ltd.) is put into alkaline solution be stirred to completely dissolve obtain alkali lignin solution, be then the rolling nanofiltration membrane circulating filtration of 1000 by above-mentioned solution molecular weight cut-off.After 2 hours, stop filtration obtaining small molecules lignin liquor, and be heated to 70 DEG C, more slowly add in above-mentioned small molecules lignin liquor mass concentration be 30% sulfuric acid carry out acid out, until filtrate pH value is 3.5.After acid out, the small molecules xylogen mixed solution obtained by above-mentioned acid out carries out centrifugation, obtains solid lignin, then solid lignin is placed in baking oven inner drying, and drying temperature is 40 DEG C, and time of drying is 8 hours, obtains dry powdery xylogen.
The powdery xylogen glycerine of above-mentioned drying is washed, filtered by glycerine, by dry in vacuum drying oven for the powdery xylogen after filtering, drying temperature is 40 DEG C again, time of drying is 3 hours, finally obtains the xylogen rubber ingredients that 16g weight-average molecular weight is less than 1000.
Embodiment 2
By 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 N23445g; 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; Xylogen rubber ingredients 2.0g prepared by this patent.
The Banbury mixer of 1L carries out mixing, calendering process is as follows:
Table 1 rubber mixing-milling technique
The rubber for tire A described in this patent is obtained after above-mentioned technique is mixing
1.
Embodiment 3
By 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 N23445g; 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; Xylogen rubber ingredients 1.0g prepared by this patent.
The Banbury mixer of 1L carries out mixing, calendering process is as follows:
Table 2 rubber mixing-milling technique
The rubber for tire A described in this patent is obtained after above-mentioned technique is mixing
2.
Embodiment 4
By 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 N23445g; 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; Xylogen rubber ingredients 5.0g prepared by this patent.
The Banbury mixer of 1L carries out mixing, calendering process is as follows:
Table 3 rubber mixing-milling technique
The rubber for tire A described in this patent is obtained after above-mentioned technique is mixing
3.
Comparative example 1
By rubber, carbon black, rubber ingredients and undressed commercially available alkali lignin (Shandong Quan Lin Chemical Co., Ltd.), carry out mixing and sulfuration according to following formula, fill a prescription as follows:
Rubber 100g; Carbon black N23445g; 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.
The Banbury mixer of 1L carries out mixing, calendering process is as follows:
Table 4 rubber mixing-milling technique
Rubber for tire B is obtained after above-mentioned technique is mixing.
Comparative example 2
By rubber, carbon black, rubber ingredients and commercially available calcium lignin sulphonate (the polynary xylogen company limited in Gaotang, Shandong), carry out mixing and sulfuration according to following formula, fill a prescription as follows:
Rubber 100g; Carbon black N23445g; 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.
The Banbury mixer of 1L carries out mixing, calendering process is as follows:
Table 5 rubber mixing-milling technique
Rubber for tire C is obtained after above-mentioned technique is mixing.
Comparative example 3
By rubber, carbon black, rubber ingredients, carry out mixing and sulfuration according to following formula, fill a prescription as follows:
Rubber 100g; Carbon black N23445g; 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 Banbury mixer of 1L carries out mixing, calendering process is as follows:
Table 6 rubber mixing-milling technique
Rubber for tire D is obtained after above-mentioned technique is mixing.
Embodiment 5
By the rubber for tire A of preparation in embodiment 2,3 and 4
1, A
2and A
3rubber for tire B, C and D of preparing with comparative example 1 ~ 3 carry out performance contrast experiment, and comparing result is as follows:
Table 7 finished composition mooney viscosity table
Table 8 finished composition mooney scorch table (125 DEG C)
Table 9 finished composition curability table (150 DEG C)
Table 10 cross-linked rubber is torn and tensile property table
Table 11 cross-linked rubber hardness performance table
Table 12 cross-linked rubber rebound performance table
Table 13 compression heat generation data sheet
Table 14DIN and Akron wear volume data sheet
Above the preparation method of a kind of xylogen rubber ingredients provided by the present invention and a kind of rubber for tire are described in detail.Apply a concrete example herein to set forth principle of the present invention and embodiment, the explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It 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 improve and modify and also fall in the protection domain of the claims in the present invention.
Claims (8)
1. a preparation method for xylogen rubber ingredients, comprises the following steps:
A) alkali lignin solution is obtained after being mixed with alkali lye by alkali lignin; 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%;
B) xylogen rubber ingredients are obtained by after the nanofiltration membrane of above-mentioned alkali lignin solution by alkaline-resisting material;
Described step B) be specially:
B1) small molecules lignin liquor is obtained by after the nanofiltration membrane of alkali lignin solution by alkaline-resisting material;
B2) by small molecules lignin liquor after acid out or spraying dry, obtain xylogen rubber ingredients;
The weight-average molecular weight of described xylogen rubber ingredients is 100 ~ 1000.
2. 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.
3. 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 DEG C.
4. a rubber for tire, is characterized in that, comprises rubber, carbon black, rubber ingredients and xylogen rubber ingredients;
Described xylogen rubber ingredients are prepared by the following method:
A) alkali lignin solution is obtained after being mixed with alkali lye by alkali lignin; 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%;
B) xylogen rubber ingredients are obtained by after the nanofiltration membrane of above-mentioned alkali lignin solution by alkaline-resisting material; Described step B) be specially: B1) obtain small molecules lignin liquor by after the nanofiltration membrane of alkali lignin solution by alkaline-resisting material; B2) by small molecules lignin liquor after acid out or spraying dry, obtain xylogen rubber ingredients; 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).
5. rubber for tire according to claim 4, is characterized in that, described carbon black is carbon black N234.
6. rubber for tire according to claim 4, is characterized in that, described rubber ingredients are rubber filling oil, latex rubber agent, activating agent for rubber, rubber antioxidant, rubber accelerator and Cure of Rubber agent.
7. rubber for tire according to claim 4, is characterized in that, described rubber filling oil is naphthenic oil; Described latex rubber 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.
8. rubber for tire according to claim 4, 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310305579.8A CN103387677B (en) | 2013-07-19 | 2013-07-19 | The preparation method of a kind of xylogen rubber ingredients and rubber for tire |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310305579.8A CN103387677B (en) | 2013-07-19 | 2013-07-19 | The preparation method of a kind of xylogen rubber ingredients and rubber for tire |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103387677A CN103387677A (en) | 2013-11-13 |
| CN103387677B true CN103387677B (en) | 2016-04-13 |
Family
ID=49532107
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310305579.8A Active CN103387677B (en) | 2013-07-19 | 2013-07-19 | The preparation method of a kind of xylogen rubber ingredients and rubber for tire |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103387677B (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105960433B (en) * | 2014-02-03 | 2018-03-30 | 株式会社普利司通 | Tire production wraps silica containing Rubber compound |
| JP6357189B2 (en) | 2015-04-24 | 2018-07-11 | 花王株式会社 | Additive for resin |
| 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 |
| 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 |
| 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1044477A (en) * | 1989-12-19 | 1990-08-08 | 华南理工大学 | Utilize the method for xylogen as rubber reinforcing filler |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5242324B2 (en) * | 2007-10-12 | 2013-07-24 | 東洋ゴム工業株式会社 | Rubber composition and pneumatic tire |
-
2013
- 2013-07-19 CN CN201310305579.8A patent/CN103387677B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1044477A (en) * | 1989-12-19 | 1990-08-08 | 华南理工大学 | Utilize the method for xylogen as rubber reinforcing filler |
Non-Patent Citations (1)
| Title |
|---|
| 碱木质素填充橡胶;潘少波等;《湖北工学院学报》;19940320;第9卷(第1期);第59-62页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103387677A (en) | 2013-11-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103387677B (en) | The preparation method of a kind of xylogen rubber ingredients and rubber for tire | |
| CN107383475B (en) | Lignin/nitrile rubber composite material and preparation method thereof | |
| CN101812191A (en) | Method for preparing polyurethane/rubber interpenetrating network type water-swellable rubber | |
| CN107892752A (en) | A kind of multi-functional lignin arylamine macromolecular antioxidant and its preparation method and application | |
| CN102796275A (en) | Method for preparing high-performance cellulose/resin composite film by UV curing process | |
| CN103923351B (en) | A kind of lignocellulose/the preparation method of polynite rubber reinforcing filler and the reinforcement of rubber | |
| CN101759885B (en) | Preparation process of water swellable rubber | |
| CN103756129A (en) | EPDM/polypropylene thermoplastic elastomer and preparation process thereof | |
| CN104558711A (en) | Rubber composite material and preparation method thereof | |
| CN104479342A (en) | Preparation method of reinforced and toughened thermoplastic polyurethane/regenerated cellulose (TPU/RC) composite film | |
| CN102234384B (en) | IPN crosslink-structure compound of tire crown rubber, mixing method and application thereof | |
| CN111196889B (en) | Multi-arm cross-linking agent and starch nanocrystal modification-based furan resin material and preparation method and application thereof | |
| CN105153462A (en) | Soybean-oil-based flame-retardant plasticizer, and preparation method and application thereof | |
| CN104194371A (en) | High-lignin-content flame-retardant polyolefin composite material and preparation method thereof | |
| CN103539912B (en) | A kind of preparation method of high-performance butadiene-styrene liquid rubber | |
| CN103525077B (en) | Surface oxidation modified vulcanized rubber powder/polyurethane composite material and preparation method thereof | |
| CN104974390B (en) | A kind of rubber water absorbent composite material containing modified wood powder | |
| CN104725648A (en) | Preparation method for degradable feather protein/sodium carboxymethylcellulose composite membrane | |
| CN102181097B (en) | Ethylene propylene diene monomer rubber sealing strip compatible with silicone adhesive | |
| CN103044691A (en) | Superfine lignin-based rubber coupling agent, manufacturing method and use thereof in rubber | |
| CN115558173B (en) | Application of industrial lignin as cutting-resistant functional auxiliary agent in preparation of cutting-resistant tire material | |
| CN112679758B (en) | Sulfur-containing copolymer cross-linked unsaturated polyester elastomer and preparation method and application thereof | |
| CN110734589A (en) | Method for preparing emulsion polymerized styrene butadiene rubber from modified graphene | |
| CN114410096B (en) | Cobalt-containing organic montmorillonite modified heat aging resistant flame retardant PC optical film material and preparation method thereof | |
| CN109206763B (en) | Chlorinated polyethylene rubber material for rubber hose and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |