CN109796603A - A kind of rubber phase solvent and preparation method thereof - Google Patents
A kind of rubber phase solvent and preparation method thereof Download PDFInfo
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- CN109796603A CN109796603A CN201811378177.XA CN201811378177A CN109796603A CN 109796603 A CN109796603 A CN 109796603A CN 201811378177 A CN201811378177 A CN 201811378177A CN 109796603 A CN109796603 A CN 109796603A
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Abstract
The invention discloses a kind of rubber phase solvents and preparation method thereof, including lignin and modifying agent, be prepared by the component of following parts by weight: lignin 70-90% and modifying agent 10-30%, preparation method include by lignin by the way that there are commonly solvent classifications and UF membrane grading technology method to be classified；Using formaldehyde, preliminary methylation modification is carried out to lignin；The modified lignin that methylates carries out compatibility modifier.The rubber phase solvent is using a large amount of lignin in the presence of nature as primary raw material, lignin has reinforcement, fire-retardant and anti-old effect in rubber, lignin, which is used, not only can preferably utilize lignin waste material in rubber, and carbon black and rubber sources can be saved, realize the high value added utilization of solid waste.The rubber phase solvent uses multiple modification during the preparation process, improves the final product quality of rubber phase solvent, so that rubber phase solvent preferably becomes the supporting material of rubber.
Description
Technical field
The present invention relates to rubber, tire and plastic products technology field, specially a kind of rubber phase solvent and its preparation side
Method.
Background technique
Rubber and plastics are important strategic materials indispensable in national economy, in people's daily life and workers and peasants
There is irreplaceable important function in industry production.Rubber and plastic filler (or mixing) be in rubber and plastic products can not
Or one of scarce most important components, dosage is huge, can not only reduce the cost of rubber and plastics, moreover it is possible to effective enhancing
The mechanics mechanical performance of final product, and assign the other functions such as conductive, thermally conductive, magnetic of rubber and plastic products.At present
The maximum rubber reinforcement filler of dosage is carbon black, and carbon black and most of rubber matrixs have excellent compatibility, have to rubber
Excellent reinforcing effect, but carbon black derives from fossil resources, is that carbon containing fossil resources (such as petroleum, natural gas, coal etc.) exist
Product obtained from the case where anoxic is not thorough burning or is thermally decomposed.Obviously, excessive dependence carbon black is unfavorable for sustainable
Development, thus it is renewable, environmental-friendly, density is small, rich reserves, rubber and plastics low in cost, that reinforcing effect is excellent are filled out
Material is always the target that vast researcher is made great efforts.
Biomass filler (or mixing) applied to polymer such as rubber and plastics mainly has cellulose, lignin, crust
Element etc. (Polymer, 2014,55,995-1003).Application outlet and market due to cellulose is extensive, the use of chitin at
This is higher, and industrial lignin is usually to be burned off power generating and heating, and the market outlet of other application is often smaller, cannot be with wood
The yield of quality matches.So how to realize that successful application of the lignin in rubber and plastic products just seems very heavy
It wants.
Lignin is one of most important ingredient of plant, it and cellulose, hemicellulose together constitute the body of plant
Dry, lignin can play the role of cohering and insect prevention.Lignin is also one of most important renewable aromatic resource,
Basic component units are three phenylpropyl alcohol alkyl structure units: p-hydroxybenzene, guaiacyl and lilac base in plant.These
Passed through C-C key or C-O key etc. between basic unit and miscellaneous be formed by connecting as three-dimensional poly- phenol macromolecular occurs
(Ind.Eng.Chem.Res.,2016,55,8691-8705).Lignin is applied in polymer material, it is undoubtedly a kind of high
Effect and high value added utilization lignin important channel, be expected to form can industrial applications new material.This aspect can solve
The certainly problem of industrial lignin resource utilization；On the other hand polymer industry is also reduced to the heavy dependence of fossil resource,
This has great significance to the sustainable development of the utilization rate, conservation of nature environment and society that improve biomass resource.Lignin
Due to reactive carboxyl and hydroxyl isoreactivity functional group in molecule, intermiscibility between lignin and many polymer with
And reactivity is by a large amount of research report, including lignin/thermoplas tic resin composite (such as polyolefin, polyvinyl chloride,
PLA, PBS, PBAT etc.), such as: application No. is a kind of lignin-epoxy resin composite material of CN201110417428.2 and
Preparation method, by epoxy resin, curing agent, toughener etc. and its homogeneous blend, passes through precompressed and heat using lignin as substrate
Cured molding obtains lignin-base composite material；Lignin/thermoset ting resin composite (mainly includes phenolic resin, ring
Oxygen resin and polyurethane etc.), such as: application No. is a kind of the water-soluble of casting low formaldehyde content of CN201810030050.2
Property phenolic resin composite and preparation method thereof, due to having used a large amount of alkali lignin in resin, can not only reduce into
This, can more be greatly reduced the burst size of formaldehyde and phenol in casting process, so that this resin is compared with similar products, more
It is environment-friendly and low-toxicity, facilitate the development that casting industry continues health；And be blended with natural rubber, such as: application No. is
A kind of preparation method of the compound modified rubber material of lignin calcium carbonate of CN201710873830.9, including following step
It is rapid: to prepare the compound of lignin calcium carbonate, Natural rubber is plasticated, mixing ingredient, rubber compound film, rubber compound film is made
Vulcanizing treatment.Organic modifier of the lignin as calcium carbonate, can be improved the intermiscibility of calcium carbonate and rubber matrix；And carbonic acid
Calcium can prevent the reunion of lignin in mixing process, promote the dispersion of lignin in the base.In short, lignin and carbonic acid
The effect of collaboration reinforcement is shown when calcium is as filler, and lignin can be improved the mechanical property of calcium carbonate in the composite
Can, there is modification to calcium carbonate；Application No. is a kind of lignin/carbon black/nitrile rubber of CN201710957263.5 is multiple
Condensation material and preparation method thereof, by being coordinated the effect of vulcanizing agent, between the segment of nitrile rubber and lignin and butyronitrile
Dynamic coordination cross-linked network is constructed between rubber phase interface, is made composite material that there is excellent comprehensive mechanical property, is overcome because of wood
Quality is poor with nitrile rubber intermiscibility and leads to the problem of physical property difference, and tensile strength can be 15~35MPa, extension at break
Rate is 250~700%；Carbon black is replaced to enhance rubber with lignin portion, it is from a wealth of sources, it is renewable, save fossil resources.
But lignin structure is complicated, the main source of industrial lignin is alkali lignin and lignosulfonate, due to being
Industrial by-product, original primary structure is degraded, and fragmentation, and molecular weight distribution is huge, leads to its usability
Can be unstable, in time with addition of coupling agent, it is also difficult to make final rubber product constant mass.Thus, at present
Until, still do not fully achieve commercialization practical application of the lignin in rubber.
Application of the lignin in the polymer such as rubber needs to realize the fine dispersion of lignin, guarantee lignin source and
The stabilization of performance, while depolarization processing, the boundary of the polymer such as Lai Zengqiang lignin and non-polar rubber are carried out to lignin
Face combines.Current lignin modification method of modifying is often only capable of improving degree of scatter of the lignin in rubber matrix, not
The interface cohesion of lignin and non-polar rubber can be significantly improved.So how to improve lignin in polymeric matrixs such as rubber
In degree of scatter and improve both intermiscibility be the key that realize lignin applied in the polymer such as rubber.
In view of the above problems, it is proposed that first to lignin carry out purifying modified, stablize its quality, then can be by it
Applied to rubber and plastic products, to realize successful application of the lignin in rubber and plastic products.The wood that we prepare
Lignin products are a kind of novel modified lignin resin products, are called lignin rubber phase solvent, it can be well dispersed in water,
And be able to achieve and be well blended and interface cohesion with natural rubber, to promote the comprehensive performance of rubber product.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the existing defects, provides a kind of rubber phase solvent and its preparation side
Method can effectively solve the problems, such as not yet to realize successful application of the lignin in rubber product in background technique.
To achieve the above object, the invention provides the following technical scheme: a kind of rubber phase solvent, including lignin and modification
Agent is prepared by the component of following parts by weight: lignin 70-90% and modifying agent 10-30%.
As a preferred technical solution of the present invention, the lignin is using Milled wood lignin, lignin by acid separation, alkali wood
One of quality, solvent lignin, lignosulfonate, oxidative lignin a variety of mix.
As a preferred technical solution of the present invention, the modifying agent includes coupling agent and surface modifier.
A kind of above-mentioned rubber phase solvent, preparation method: includes the following steps:
S1, classification: by lignin by the way that there are commonly solvent classifications and UF membrane grading technology method to be classified, make
Lignin molecular weight more evenly, molecular weight be 1-3 ten thousand；
S2, the lignin after step S1 classification be modified step by step:
A, using formaldehyde, preliminary methylation modification is carried out to lignin；
B, the modified lignin that methylates carries out intermiscibility and is modified, specific method, with coupling agent, non-ionic surface active
Agent is modified, and temperature controls in the range of 60-150 DEG C, modification time is about 20 minutes, the pressure inside modifying machine should be controlled
In the range of 0-0.4MPa, modified-reaction carries out system in common solvent, the mass concentration control of lignin in modifying process
Between 1-30%；
S3, will by the modified lignin of branch be delivered to granulation machinery in carry out granulation processing；
S4, will graininess lignin is transferred in drying equipment by being granulated that treated is dried, drying is set
Standby drying temperature should control in the range of 100-130 DEG C, and drying time controlled in the range of 2-5 hours；
S5, the granular lignin after drying and processing is subjected to packing processes, be finally transferred in warehouse, complete entire preparation
Process.
It is used during modified twice-modified of step S2 distribution as a preferred technical solution of the present invention
Solvent includes DMSO, DMF, DMAC, ionic liquid and eutectic solvent.
Compared with prior art, the beneficial effects of the present invention are: the rubber phase solvent is using big in the presence of nature
The lignin of amount is advantageous in that as primary raw material using lignin: lignin has reinforcement, fire-retardant and anti-old in rubber
Lignin is used and not only can use lignin waste material in rubber, but also can save carbon black and rubber sources by effect, real
The high value added utilization of existing solid waste, in addition, the lignin rubber phase solvent (modified lignin resin) is adopted during the preparation process
With multiple modification, the final product quality of rubber phase solvent is improved, rubber phase solvent is enabled preferably to become the benefit of rubber
Strong filler.The highest dosage of lignin rubber phase solvent can account for the 50% of natural rubber, so as to reduce cost, and take turns
The formula system of tire does not need to do big adjustment.In addition, the phase solvent product can not only be added to rubber in the form of auxiliary agent
It is used in plastics, can also be used to that production multifunctional constant viscose glue is blended by wet process with natural rubber.
Detailed description of the invention
Fig. 1 is that the RPA2000 anaerobic ageing properties of the embodiment of the present invention 4 detect figure.
Specific embodiment
The present invention provides a kind of technical solution: a kind of rubber phase solvent, including lignin and modifying agent, by following parts by weight
Component be prepared: lignin 70-90% and modifying agent 10-30%.
Lignin is using Milled wood lignin, lignin by acid separation, alkali lignin, solvent lignin, lignosulfonate, oxidation wood
One of quality a variety of mixes.
Modifying agent includes coupling agent and surface modifier.
Preferably, the rubber phase solvent, in the preparation: including the following steps:
S1, classification: by lignin by the way that there are commonly solvent classifications and UF membrane grading technology method to be classified, make
Lignin molecular weight more evenly, molecular weight be 1-3 ten thousand；
S2, the lignin after step S1 classification be modified step by step:
A, using formaldehyde, preliminary methylation modification is carried out to lignin；
B, the modified lignin that methylates carries out intermiscibility and is modified, specific method, with coupling agent, non-ionic surface active
Agent is modified, and temperature controls in the range of 60-150 DEG C, modification time is about 20 minutes, the pressure inside modifying machine should be controlled
In the range of 0-0.4MPa, modified-reaction carries out system in common solvent, and the mass concentration control of lignin exists in modifying process
Between 1-30%；
S3, will by the modified lignin of branch be delivered to granulation machinery in carry out granulation processing；
S4, will graininess lignin is transferred in drying equipment by being granulated that treated is dried, drying is set
Standby drying temperature should control in the range of 100-130 DEG C, and drying time controls in 2-5 hours ranges；
S5, the granular lignin after drying and processing is subjected to packing processes, be finally transferred in warehouse, complete entire preparation
Process.
During modified twice-modified of step S2 distribution, common solvent includes DMSO, DMF, DMAC, ionic liquid and low
Congruent melting solvent.
Embodiment 1
A kind of rubber phase solvent is made after grading purification and modifier modification by lignin.
Lignin used in this example is Milled wood lignin, and specific modification procedure is as follows:
S1, classification: Milled wood lignin is dispersed in ethanol solution, 2000rpm centrifugal sedimentation 5 minutes, can be divided into
Solvable lignin and insoluble lignin will carry out the modification of next step after 90 degree of insoluble lignin drying；After classification not
Molten lignin average molecular weight is about 2.8 ten thousand, molecular weight distribution index 1.6.
S2, the lignin after step S1 classification be modified step by step:
A, using formaldehyde, preliminary methylation modification (step is conventional methylated modification) is carried out to lignin；
B, the modified lignin that methylates carries out intermiscibility and is modified, and specific method, lignin quality score accounts for 90%, uses
It is 4% that silane coupling agent mass fraction, which accounts for 6%, non-ionic surfactant Tween, 80 mass fraction, is modified, temperature control
120 DEG C, modification time are 20 minutes, the pressure inside modifying machine should be controlled in 0.1MPa, modified-reaction is in DMSO solvent
It carries out, the mass concentration of lignin is controlled 10% in modifying process；
S3, separation of solid and liquid recycling design will be carried out by the modified lignin of branch, modified lignin does not dissolve in
Modified lignin is delivered in granulation machinery and carries out granulation processing by DMSO；
S4, will graininess lignin is transferred in drying equipment by being granulated that treated is dried, drying is set
Standby drying temperature should be controlled at 100 DEG C, and drying time was controlled at 4 hours；
S5, the granular lignin after drying and processing is subjected to packing processes, be finally transferred in warehouse, complete entire preparation
Process.Obtained product is lignin rubber phase solvent product, and product inorganic content is less than 3%.
Embodiment 2
A kind of rubber phase solvent is made after grading purification and modifier modification by lignin.
Lignin used in this example is alkali lignin, and specific modification procedure is as follows:
S1, classification: alkali lignin is soluble in water, and tune pH value is faintly acid, and lignin deposit is precipitated, and film filters solid-liquid
The lignin of precipitating is dispersed in acetone soln again after separation, 2000rpm centrifugal sedimentation 8 minutes, solvable wood can be divided into
Quality and insoluble lignin will carry out the modification of next step after 80 degree of insoluble lignin drying；It is insoluble wooden after classification
Plain average molecular weight is about 1.2 ten thousand, molecular weight distribution index 1.4.
S2, the lignin after step S1 classification be modified step by step:
A, using formaldehyde, preliminary methylation modification (step is conventional methylated modification) is carried out to lignin；
B, the modified lignin that methylates carries out intermiscibility and is modified, and specific method, lignin quality score accounts for 80%, uses
Silane coupling agent mass fraction accounts for 3%, aluminum-zirconium coupling agent mass fraction and accounts for 2%, 20 mass of non-ionic surfactant Tween point
Number is 5%, is modified, and temperature control is 130 DEG C, modification time are 18 minutes, the pressure inside modifying machine should control
0.2MPa, modified-reaction carry out in DMF solvent, and the mass concentration of lignin is controlled 15% in modifying process；
S3, separation of solid and liquid recycling design will be carried out by the modified lignin of branch, modified lignin does not dissolve in
Modified lignin is delivered in granulation machinery and carries out granulation processing by DMF；
S4, will graininess lignin is transferred in drying equipment by being granulated that treated is dried, drying is set
Standby drying temperature should be controlled at 110 DEG C, and drying time was controlled at 3.5 hours；
S5, the granular lignin after drying and processing is subjected to packing processes, be finally transferred in warehouse, complete entire preparation
Process.Obtained product is lignin rubber phase solvent product, and product inorganic content is less than 3%.
Embodiment 3
A kind of rubber phase solvent is made after grading purification and modifier modification by lignin.
Lignin used in this example is the solvent lignin that formic acid method is isolated, and specific modification procedure is as follows:
S1, classification: solvent lignin is dispersed in methanol solution, 3000rpm centrifugal sedimentation 5 minutes, can be divided into
Solvable lignin and insoluble lignin will carry out the modification of next step after 90 degree of insoluble lignin drying；After classification not
Molten lignin average molecular weight is about 2.9 ten thousand, molecular weight distribution index 1.2.
S2, the lignin after step S1 classification be modified step by step:
A, using formaldehyde, preliminary methylation modification (step is conventional methylated modification) is carried out to lignin；
B, the modified lignin that methylates carries out intermiscibility and is modified, and specific method, lignin quality score accounts for 85%, uses
Silane coupling agent mass fraction accounts for 4%, aluminum-zirconium coupling agent mass fraction and accounts for 1%, 20 mass of non-ionic surfactant Tween point
Number is 3%, and nonionic surfactant Span60 mass fraction 2% is modified, and temperature control is in 135 DEG C, modification time
20 minutes, the pressure inside modifying machine should control in 0.22MPa, modified-reaction carries out in DMAC solvent, wooden in modifying process
The mass concentration of quality is controlled 20%；
S3, separation of solid and liquid recycling design will be carried out by the modified lignin of branch, modified lignin does not dissolve in
Modified lignin is delivered in granulation machinery and carries out granulation processing by DMAC；
S4, will graininess lignin is transferred in drying equipment by being granulated that treated is dried, drying is set
Standby drying temperature should be controlled at 120 DEG C, and drying time was controlled at 3.5 hours；
S5, the granular lignin after drying and processing is subjected to packing processes, be finally transferred in warehouse, complete entire preparation
Process.Obtained product is lignin rubber phase solvent product, and product inorganic content is less than 2%.
Embodiment 4 (Application Example)
This application embodiment is that the products application that obtains embodiment 3 is encapsulated in dumbbell.
1# dumbbell encapsulation formulation: 3# mark glue, 80 parts；SBR1502,20 parts；Zinc oxide, 5 parts；Stearic acid, 2 parts； N330
50 parts；Calcium carbonate, 70 parts；4# white oil, 23 parts；Antioxidant 4010,1.5 parts；Sulphur, 2.1 parts；
2# dumbbell encapsulation formulation: 3# mark glue, 80 parts；SBR1502,20 parts；Zinc oxide, 5 parts；Stearic acid, 2 parts； N330
50 parts；Calcium carbonate, 70 parts；4# white oil, 23 parts；Antioxidant 4010,1.5 parts；Sulphur, 2.1 parts；The additional embodiment 3 that is added obtains
5 parts of lignin rubber phase solvent product.
Rheology testing/MDR (test condition: 145 DEG C × 50 minutes)
| It is interior | Cpd | ML | MH/ | TS1 | TS | T10 | T5 | T9 |
| 1# | 41. | 0. | 4.5 | 6.3 | 7. | 8.0 | 9. | 10 |
| 2# | 40. | 0. | 4.6 | 6.5 | 7. | 8.1 | 9. | 10 |
It is little to fill 5 parts of rubber phase solvents rheological property difference encapsulated with normality dumbbell, minimal torque fall compared with
Greatly, mold filling performance is more excellent.
The test of rubber compound stress relaxation
| Sample | ML1+4 | tx80( | Intercept | slope( | Relaxation area |
| 1# | 41.3 | 19.35 | 21.23 | -0.307 | 841 |
| 2# | 40.5 | 20.09 | 20.93 | -0.315 | 807 |
General stress relaxation area is smaller, and the extrusion mouth-type expansion of sizing material is smaller, and the processing performance of sizing material is more excellent, and characterization is mixed
It is more excellent to refine the processing performances such as characteristic, extrusion dimensional stability.So 2# fills 5 parts of rubber phase solvent ratio 1# normality dumbbell stress
Relaxation property is more excellent.
Physical mechanical property (conditions of vulcanization: 137 DEG C, 25 minutes)
5 parts of encapsulated physical mechanical properties of rubber phase solvent ratio 1# normality dumbbell of 2# filling are more excellent, and breaking strength improves
26%.
Resilience, hardness, abrasivity test
Hardness, tearing strength are substantially suitable；2# resilience is encapsulated better than the normality dumbbell that 1# is not added with rubber phase solvent；Mill
Consumption can be more excellent, and abrasion loss reduces by 16%.
Test results are shown in figure 1 for RPA2000 anaerobic ageing properties.
It is tested using RPA2000, observes the variable quantity of the tan δ before and after heat ageing, measure the heat-resistant aging of vulcanizate
Can, it makes a variation smaller, illustrates that the ageing properties of vulcanizate are better, 2# fills 5 parts of rubber phase solvent products as can be seen from the above table
It is encapsulated that ageing properties are substantially better than 1# normality dumbbell.
So fill 5 parts of rubber phase solvents compared with normality dumbbell is encapsulated, rheological property, elongation at break, hardness torn
Substantially suitable in terms of splitting, breaking strength, wear hardness, resilience etc. are more excellent；Adding 5 parts of rubber phase solvents can effectively reduce
Aggtegation between filler increases the interaction between polymer and filler.Filling modifying agent T1202 answering in dumbbell is encapsulated
With can shorten the fillers such as carbon black and be mixed into the time, reduce and be kneaded energy consumption, amount of filler can be greatly increased, reduce the encapsulated cost of dumbbell.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.Any reference signs in the claims should not be construed as limiting the involved claims.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (5)
1. a kind of rubber phase solvent, including lignin and modifying agent, it is characterised in that: by the component preparation of following parts by weight
: lignin 70-90% and modifying agent 10-30%.
2. a kind of rubber phase solvent according to claim 1, it is characterised in that: the lignin using Milled wood lignin,
One of lignin by acid separation, alkali lignin, solvent lignin, lignosulfonate, oxidative lignin a variety of mix.
3. a kind of rubber phase solvent according to claim 1, it is characterised in that: the modifying agent includes coupling agent and surface
Modifying agent.
4. any one rubber phase solvent described in -3 according to claim 1, preparation method: includes the following steps:
S1, classification: by lignin by the way that there are commonly solvent classifications and UF membrane grading technology method to be classified, so that wooden
More evenly, molecular weight is 1-3 ten thousand to the molecular weight of quality；
S2, the lignin after step S1 classification be modified step by step:
A, using formaldehyde, preliminary methylation modification is carried out to lignin；
B, it is modified that the modified lignin of methylating carries out intermiscibility, specific method, with coupling agent, nonionic surfactant into
Row is modified, and temperature controls in the range of 60-150 DEG C, modification time is about 20 minutes, the pressure inside modifying machine should control
In the range of 0-0.4MPa, modified-reaction is carried out in common solvent, and the mass concentration of lignin is controlled in 1- in modifying process
Between 30%；
S3, will by the modified lignin of branch be delivered to granulation machinery in carry out granulation processing；
S4, will graininess lignin is transferred in drying equipment by being granulated that treated is dried, drying equipment
Drying temperature should control in the range of 100-130 DEG C, and drying time controlled in the range of 2-5 hours；
S5, the granular lignin after drying and processing is subjected to packing processes, be finally transferred in warehouse, completion was entirely prepared
Journey.
5. a kind of rubber phase solvent according to claim 4 and preparation method thereof, it is characterised in that: the step S2 distribution
It is modified it is twice-modified during, common solvent include one of DMSO, DMF, DMAC, ionic liquid and eutectic solvent or
It is several.
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| CN116178976A (en) * | 2023-02-21 | 2023-05-30 | 上海昶法新材料有限公司 | Preparation method of modified lignin and application of modified lignin in natural rubber |
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Application publication date: 20190524 |