CN107446220A - A kind of preparation method of enzymolysis xylogen plastic composite - Google Patents
A kind of preparation method of enzymolysis xylogen plastic composite Download PDFInfo
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- CN107446220A CN107446220A CN201710875207.7A CN201710875207A CN107446220A CN 107446220 A CN107446220 A CN 107446220A CN 201710875207 A CN201710875207 A CN 201710875207A CN 107446220 A CN107446220 A CN 107446220A
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- enzymolysis xylogen
- composite
- enzymolysis
- dried
- xylogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G1/00—Lignin; Lignin derivatives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2397/00—Characterised by the use of lignin-containing materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
A kind of preparation method of enzymolysis xylogen plastic composite, belongs to plastic composite technical field, comprises the following steps：Prepare enzymolysis xylogen, the processing of enzymolysis xylogen air-flow crushing, mixed material is made in addition auxiliary agent, composite filler particles are made in addition calcium carbonate, material is kneaded.The grain diameter that the present invention handles to obtain by air-flow crushing is smaller, and average grain diameter is 3 μm ± 0.1 μm, and enzymolysis xylogen grain diameter is smaller, and the tensile strength of composite is bigger.It is favorably improved the mechanical property of composite.The present invention is by adding plastic additive：Dioctyl phthalate, silane coupler and calcium stearate improve the interface compatibility between enzymolysis xylogen and polyvinyl resin, improve the lubrication between enzymolysis xylogen molecule and polyethylene molecular chain, improve the comprehensive mechanical property of composite.
Description
Technical field
The invention belongs to plastic composite technical field, and in particular to a kind of system of enzymolysis xylogen plastic composite
Preparation Method.
Background technology
Polyvinyl resin due to it is cheap, performance is good, as the continuous development of technology, polyethylene are excellent with its
Mechanical performance and chemical stability, it is widely used in each sides such as industry, agricultural, medicine, health and daily living article
Face, have become the kind that yield is maximum in plastic resin.In most cases, polyvinyl resin is not single use
, but want mixed filler.Filler, also known as filler, he is for improving the performance of vinyon product, reducing product
Cost, have very significant effect.Due to filler wide material sources, cheap, so being processed in vinyon
In have a wide range of applications.But solving filler and polyvinyl resin compatibility at present, improving the side such as composite materials property
Face need further to improve.
The content of the invention
In order to solve problems of the prior art, do invention and provide a kind of enzymolysis xylogen plastic composite
Preparation method, it is intended that improve the compatibility of filler and polyvinyl resin, filler in polyvinyl resin be evenly distributed degree and
Improve composite materials property.
In order to solve problems of the prior art, the present invention uses following technical scheme：
A kind of preparation method of enzymolysis xylogen plastic composite, comprises the following steps：
Step 1：10g enzymolysis maize straw residues are added in the sodium hydroxide solution of 160mL mass concentrations 3%, 65
To be filtered after DEG C stirring reaction 1.5h, filtrate adjusts pH to 3 with the dilute sulfuric acid of mass concentration 2%, is then incubated 30min at 70 DEG C,
Centrifuged after being stored at room temperature overnight, precipitation is cleaned after 60 DEG C of dryings to enzymolysis xylogen with water；
Step 2：Enzymolysis xylogen 150g is weighed to be positioned in container, it is continuous in 80 DEG C, 80bar vacuum drying chamber
24h is dried, a sample is stirred every 12h, is sealed after taking-up standby；
Step 3：Air-flow crushing processing is carried out to the sample, air-flow crushing, control are carried out using BPQ-50 airslide disintegrating mills
Sample preparation product charging rate is 300g/h, and it is 0.6MPa, exit pressure 0.6MPa to crush air inlet pressure；
Step 4：Enzymolysis xylogen after crushing is positioned in 80 DEG C of thermostatic drying chamber processing is dried, dried
After 24h, it is standby to take out sealing；
Step 5：The enzymolysis xylogen for weighing dried 20g is laid on surface plate, with rubber head dropper by 7.5g neighbour's benzene
Diformazan dioctyl phthalate disperses to be added on enzymolysis xylogen dropwise, and adds 3g silane couplers and 3g calcium stearates, and stirring is equal
After even, taken out after mixing 1min using mixed at high speed crusher in crushing, 24h is dried in 80 DEG C of thermostatic drying chambers and is taken out, is obtained mixed
Compound material；
Step 6：Mixed material 10g and calcium carbonate 10g is weighed, 200ml water is added, is stirred using magnetic stirring apparatus,
Suspension system is become, suspension is spray-dried, sets vapo(u)rizing temperature as 180 DEG C, outlet temperature is 90 DEG C, spraying
Speed is 6ml/min, obtain composite filler particles, in 80 DEG C of thermostatic drying chambers dry 24h after take out it is standby；
Step 7：Weigh high density polyethylene materials particle 300g to be positioned in container, done in the vacuum of 80 DEG C, 80bar
Continuous drying 24h in dry case, a sample is stirred every 12h, is sealed after taking-up standby；
Step 8：The high density polyethylene materials particle of 80 dry parts by weight is weighed, rubber mixing machine is preheated, when double roller temperature
When reaching 170 DEG C high density polyethylene materials are carried out with refining glue, after 2min, adds its mass percent 20wt% compound filling out
Material particle is kneaded, and after being kneaded 10min, obtains composite.
Preferably, the average grain diameter for enzymolysis xylogen being obtained after the processing of described step three alkali air-flow crushing is 3 μm of ± 0.1 μ
m。
Preferably, the rubber mixing machine described in step 8 is the open refining glue molding machines of X (S) K.
Described enzymolysis maize straw residue produces for COFCO.
The beneficial effects of the present invention are:
1) alkaline aqueous solution extraction is used, extracts enzymolysis xylogen from enzymolysis maize straw residue, yield reaches
20%, it has typical draft class lignin structure.
2) grain diameter that the present invention handles to obtain by air-flow crushing is smaller, and average grain diameter is 3 μm ± 0.1 μm, enzymolysis
Lignin particles particle diameter is smaller, and the tensile strength of composite is bigger.It is favorably improved the mechanical property of composite
3) present invention is by adding plastic additive：Dioctyl phthalate, silane coupler and calcium stearate improve
Interface compatibility between enzymolysis xylogen and polyvinyl resin, improve between enzymolysis xylogen molecule and polyethylene molecular chain
Lubrication, improve the comprehensive mechanical property of composite.
4) organic modifier of the lignin as calcium carbonate, the compatibility of calcium carbonate and base polyethylene can be improved；And
Calcium carbonate can prevent the reunion of lignin in mixing process, promote lignin in the base scattered.In a word, lignin and
The effect of synergistic reinforcement is shown when calcium carbonate is as filler, and lignin can improve the power of calcium carbonate in the composite
Performance is learned, there is modification to calcium carbonate.
Embodiment
Below by the description to embodiment, the present invention is further detailed explanation, to help people in the art
Member has more complete, accurate and deep understanding to inventive concept of the invention, technical scheme.
Embodiment 1
A kind of preparation method of enzymolysis xylogen plastic composite, comprises the following steps：
Step 1：10g enzymolysis maize straw residues are added in the sodium hydroxide solution of 160mL mass concentrations 3%, 65
To be filtered after DEG C stirring reaction 1.5h, filtrate adjusts pH to 3 with the dilute sulfuric acid of mass concentration 2%, is then incubated 30min at 70 DEG C,
Centrifuged after being stored at room temperature overnight, precipitation is cleaned after 60 DEG C of dryings to enzymolysis xylogen with water；
Step 2：Enzymolysis xylogen 150g is weighed to be positioned in container, it is continuous in 80 DEG C, 80bar vacuum drying chamber
24h is dried, a sample is stirred every 12h, is sealed after taking-up standby；
Step 3：Air-flow crushing processing is carried out to the sample, air-flow crushing, control are carried out using BPQ-50 airslide disintegrating mills
Sample preparation product charging rate is 300g/h, and it is 0.6MPa, exit pressure 0.6MPa to crush air inlet pressure；
Step 4：Enzymolysis xylogen after crushing is positioned in 80 DEG C of thermostatic drying chamber processing is dried, dried
After 24h, it is standby to take out sealing；
Step 5：The enzymolysis xylogen for weighing dried 20g is laid on surface plate, with rubber head dropper by 7.5g neighbour's benzene
Diformazan dioctyl phthalate disperses to be added on enzymolysis xylogen dropwise, and adds 3g silane couplers and 3g calcium stearates, and stirring is equal
After even, taken out after mixing 1min using mixed at high speed crusher in crushing, 24h is dried in 80 DEG C of thermostatic drying chambers and is taken out, is obtained mixed
Compound material；
Step 6：Mixed material 10g and calcium carbonate 10g is weighed, 200ml water is added, is stirred using magnetic stirring apparatus,
Suspension system is become, suspension is spray-dried, sets vapo(u)rizing temperature as 180 DEG C, outlet temperature is 90 DEG C, spraying
Speed is 6ml/min, obtain composite filler particles, in 80 DEG C of thermostatic drying chambers dry 24h after take out it is standby；
Step 7：Weigh high density polyethylene materials particle 300g to be positioned in container, done in the vacuum of 80 DEG C, 80bar
Continuous drying 24h in dry case, a sample is stirred every 12h, is sealed after taking-up standby；
Step 8：The high density polyethylene materials particle of 80 dry parts by weight is weighed, rubber mixing machine is preheated, when double roller temperature
When reaching 170 DEG C high density polyethylene materials are carried out with refining glue, after 2min, adds its mass percent 20wt% compound filling out
Material particle is kneaded, and after being kneaded 10min, obtains composite.
The average grain diameter that enzymolysis xylogen is obtained after described step three alkali air-flow crushing processing is 3 μm ± 0.1 μm.
Rubber mixing machine described in step 8 is the open refining glue molding machines of X (S) K.
Described enzymolysis maize straw residue produces for COFCO.
Claims (3)
1. a kind of preparation method of enzymolysis xylogen plastic composite, it is characterised in that comprise the following steps：
Step 1：10g enzymolysis maize straw residues are added in the sodium hydroxide solution of 160mL mass concentrations 3%, stirred at 65 DEG C
Filtered after mixing reaction 1.5h, filtrate adjusts pH to 3 with the dilute sulfuric acid of mass concentration 2%, is then incubated 30min, room temperature at 70 DEG C
Centrifuged after standing overnight, precipitation is cleaned after 60 DEG C of dryings to enzymolysis xylogen with water；
Step 2：Weigh enzymolysis xylogen 150g to be positioned in container, the continuous drying in 80 DEG C, 80bar vacuum drying chamber
24h, a sample is stirred every 12h, is sealed after taking-up standby；
Step 3：Air-flow crushing processing is carried out to the sample, air-flow crushing is carried out using BPQ-50 airslide disintegrating mills, controls sample
Product charging rate is 300g/h, and it is 0.6MPa, exit pressure 0.6MPa to crush air inlet pressure；
Step 4：Enzymolysis xylogen after crushing is positioned in 80 DEG C of thermostatic drying chamber processing is dried, dry 24h
Afterwards, it is standby to take out sealing；
Step 5：The enzymolysis xylogen for weighing dried 20g is laid on surface plate, with rubber head dropper by 7.5g O-phthalics
Dioctyl phthalate disperses to be added on enzymolysis xylogen dropwise, and adds 3g silane couplers and 3g calcium stearates, after stirring,
Taken out after mixing 1min using mixed at high speed crusher in crushing, 24h is dried in 80 DEG C of thermostatic drying chambers and is taken out, obtains mixture
Material；
Step 6：Mixed material 10g and calcium carbonate 10g is weighed, 200ml water is added, is stirred, made into using magnetic stirring apparatus
For suspension system, suspension is spray-dried, sets vapo(u)rizing temperature as 180 DEG C, outlet temperature is 90 DEG C, spray velocity
For 6ml/min, obtain composite filler particles, dried in 80 DEG C of thermostatic drying chambers take out after 24h it is standby；
Step 7：Weigh high density polyethylene materials particle 300g to be positioned in container, in 80 DEG C, 80bar vacuum drying chamber
Middle continuous drying 24h, a sample is stirred every 12h, is sealed after taking-up standby；
Step 8：The high density polyethylene materials particle of 80 dry parts by weight is weighed, rubber mixing machine is preheated, when double roller temperature reaches
Refining glue is carried out to high density polyethylene materials at 170 DEG C, after 2min, adds its mass percent 20wt% compounded mix
Grain is kneaded, and after being kneaded 10min, obtains composite.
A kind of 2. preparation method of enzymolysis xylogen plastic composite according to claim 1, it is characterised in that：It is described
The step of three alkali air-flow crushings processing after enzymolysis xylogen average grain diameter be 3 μm ± 0.1 μm.
A kind of 3. preparation method of enzymolysis xylogen plastic composite according to claim 1, it is characterised in that：Step
Rubber mixing machine described in eight is the open refining glue molding machines of X (S) K.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710875207.7A CN107446220A (en) | 2017-09-25 | 2017-09-25 | A kind of preparation method of enzymolysis xylogen plastic composite |
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| CN201710875207.7A CN107446220A (en) | 2017-09-25 | 2017-09-25 | A kind of preparation method of enzymolysis xylogen plastic composite |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103224661A (en) * | 2013-04-26 | 2013-07-31 | 华南理工大学 | Polyolefin/enzymatic-hydrolyzed lignin composite material and preparation method thereof |
| CN104356663A (en) * | 2014-12-03 | 2015-02-18 | 松原光禾能源有限公司 | Preparation method of lignin thermoplastic material |
| CN104371341A (en) * | 2014-12-03 | 2015-02-25 | 松原光禾能源有限公司 | Preparation method of lignin thermoplastic material |
| CN106349534A (en) * | 2016-08-22 | 2017-01-25 | 华南理工大学 | Enzymatic hydrolysis lignin/polyolefin composite material as well as preparation method and application thereof |
-
2017
- 2017-09-25 CN CN201710875207.7A patent/CN107446220A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103224661A (en) * | 2013-04-26 | 2013-07-31 | 华南理工大学 | Polyolefin/enzymatic-hydrolyzed lignin composite material and preparation method thereof |
| CN104356663A (en) * | 2014-12-03 | 2015-02-18 | 松原光禾能源有限公司 | Preparation method of lignin thermoplastic material |
| CN104371341A (en) * | 2014-12-03 | 2015-02-25 | 松原光禾能源有限公司 | Preparation method of lignin thermoplastic material |
| CN106349534A (en) * | 2016-08-22 | 2017-01-25 | 华南理工大学 | Enzymatic hydrolysis lignin/polyolefin composite material as well as preparation method and application thereof |
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Application publication date: 20171208 |
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