CN108219499A - A kind of preparation method for the wood fibre for optimizing wood plastic composite preparation process - Google Patents
A kind of preparation method for the wood fibre for optimizing wood plastic composite preparation process Download PDFInfo
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- CN108219499A CN108219499A CN201810030867.XA CN201810030867A CN108219499A CN 108219499 A CN108219499 A CN 108219499A CN 201810030867 A CN201810030867 A CN 201810030867A CN 108219499 A CN108219499 A CN 108219499A
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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
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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
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Abstract
The invention discloses a kind of preparation methods for the wood fibre for optimizing wood plastic composite preparation process.Method uses polyhexamethylene guanide phosphate solution respectively, and graphite oxide microplate is attached to the surface of wood fibre by electrostatic interaction, controls reaction process by adjusting the pH value of reaction and the temperature of reaction, realizes the preparation of product.There is good lubricating action by wood fibre prepared by this method, small with the rubbing action of machine barrel and rotor or screw rod, friction heat release is few, and wood fibre is not easy coking in the process of Wood-plastic material, its heat resistance is strengthened, and meets the use demand of wood plastic composite.
Description
Technical field
The invention belongs to natural wooden fibers to be modified field, relates to a kind of wood for optimizing wood plastic composite preparation process
The preparation method of matter fiber.
Technical background
Wood plastic composite is a kind of by plastics and plant fiber or wooden powder, by melt blending, then through squeezing,
Bio-based materials prepared by the forming methods such as molding, injection moulding.Because have raw material resources, environmentally friendly renewable, specific strength compared with
The advantages that high, price market and product plasticization, wood plastic composite is just increasingly extensive to be applied to building materials, automobile and household
The key areas such as electric appliance.Wood plastic composite not only effectively alleviates the resource problem that China is short of timber, but also complete as solving
The important channel of ball environmental problems such as " white pollution " caused by plastics are widely used.Therefore, wood plastic composite has
Huge application value and prospect, particularly in recent years, demand average growth rate per annum are more than 20%, in building materials and auto industry
Wait the increasingly increase of domain requirements amount.However, the various technical problems in its process are also to be solved, for example squeezed in wood moulding
During going out section bar, extrusion wild effect is often had, defect rate and rejection rate are higher；Wood fibre is in wood and plastic composite
It is unevenly distributed in material, the process equipment loss of wood plastic composite is higher.
Wood fibre is the fibre-like extracted from bamboo and wood or the industrial wood waste matter of other natural materials
Substance；It is derived from a wealth of sources, cheap and environmental-friendly, is widely used in producing all kinds of wood plastic composites.However, by wooden
During matter fiber and processing of high molecular material are wood plastic composite, especially with form processing is squeezed out, largely quickly
When squeezing out various Wood-plastic profiles, two-phase in the poor product that can cause to squeeze out of interfacial adhesion between wood fibre and plastics
It is unevenly distributed, so as to influence quality of item.In this case, it if adding in a large amount of interfacial compatibilizer in formula, plays
Effect it is also extremely limited, and the production cost of product can be greatlyd improve..In addition, the wood fibre surface largely added in
Hydrogen bond is formed with a large amount of hydroxyl, the viscosity rising and mobility that can lead to melt in process decline.
Since the heat-conductive characteristic of wood fibre and plastics is all poor, when wood fibre and screw rod or machine tube inner wall part
When friction heat release or in the case where the temperature slightly higher residence time is long, wood fibre, which has, there is local coking
Phenomenon, it is final so that the phenomenon that part blacks occurs in the wood plastic composite prepared.
Invention content
In order to solve the problems, such as background technology, the present invention proposes a kind of optimization wood plastic composite preparation process
Wood fibre preparation method, by the wood fibre prepared by this method, since its surface is born by electrostatic interaction
Graphene oxide microplate is carried so that wood fibre can optimize the machined parameters of wood plastic composite in process, carry
The quality of high wood plastic composite.
The technical solution adopted by the present invention to solve the technical problems is to comprise the steps of：
Graphene oxide microplate and polyelectrolyte are carried out LBL self-assembly, by oxygen by the present invention by electrostatic interaction
Graphite alkene microplate is carried on the surface layer of wood fibre.Due to the lubricating action of graphene microchip, can greatly reduce wooden
Friction between fiber and screw rod and machine tube inner wall；Graphene microchip can effectively improve the heat resistance of wood fibre, so as to
The phenomenon that local coking being effectively prevented in process.
The wood fibre being prepared by the method for the present invention can effectively improve the mobility of the melt of wood plastic composite
Reduce the rubbing action of melt and machine barrel and rotor or screw rod, reduce friction heat release so that wood fibre is in Wood-plastic material
Process is not easy coking, and heat resistance is strengthened, and meets the use demand of wood plastic composite.
The beneficial effects of the invention are as follows：
(1) wood fibre prepared by the present invention, can natural degradation in the environment, be environment friendly material.
(2) present invention prepares the process of wood fibre, and using aqueous reaction system, reaction reagent is environmentally protective, reacts
Journey is rapidly and efficiently；
(3) wood fibre prepared by the present invention can effectively improve its melt during Screw for Manufacturing Wood-plastic Composite
Mobility, reduce the rubbing action of melt and machine barrel and rotor or screw rod；
(4) the wood fibre heat resistance enhancing prepared by the present invention, the phenomenon that being not susceptible to local coking, production is more high-quality
Wood plastic product.
Specific embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but should not this be interpreted as this hair
Bright range is only limitted to example.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
The embodiment of the present invention is as follows：
Embodiment 1：
Step 1：The polyhexamethylene guanide phosphate solution of 25wt% is diluted to the aqueous solution of 5wt%, adds in hydroxide
Sodium solution, by its pH value adjustment to 10.5, labeled as solution A；By graphite oxide microplate, distilled water is added in, is kept for 50 DEG C, ultrasound
5min prepares the aqueous solution of 2.5wt%, adds in aqueous hydrochloric acid solution, is 2.7 by pH value adjustment, labeled as B solution.
Step 2：20g wood fibres are weighed, in the solution A of 100ml, 10~15min of ultrasound at 70 DEG C, strainer filtering,
Quick-air-drying at 80 DEG C；In the B solution of 100ml, 5~10min of ultrasound at 75 DEG C, strainer filtering, Quick-air-drying at 80 DEG C；Weight
Aforesaid operations 5 times again are placed in 105 DEG C of baking oven dry 2h and obtain wood fibre, labeled as modified wood fibre -1.
The heat decomposition curve of wood fibre is analyzed with thermogravimetry, the starting of obtained modified wood fibre -1
Decomposition temperature is：174℃；Maximum decomposition temperature：372℃；(initial decomposition temperature of initial wood mass fiber is：159℃；It is maximum
Decomposition temperature：361℃).As it can be seen that the thermal stability of modified wood fibre -1 is better than initial wood mass fiber.
Due to torque rheometer, structure is similar, and material amounts are few with actual production equipment (mixer, extruder etc.), institute
The processes such as mixing, extrusion can be simulated in the lab, particularly suitable for optimization factory formula and process conditions.Haake torque rheology
The energy that instrument records reaction torque and release of the material to rotor or screw rod generation in mixed process changes with time, wherein
Counter balance torque value and material molten after melt viscosity and mobility it is corresponding.Counter balance torque value is lower, and material is being sheared
Under effect, viscosity when reaching melt stability is lower, and mobility during processing is better.By wood fibre, polypropylene (PP)
And maleic anhydride inoculated polypropylene is with 20:75:5 weight percent, at 170 DEG C, rotor speed 30rad/min, with Kazakhstan
Gram torque rheology instrument carries out melt blending, and following parameter is recorded automatically during melt blending：Haake torque rheology instrument
The energy (E) released in the torque (M) and Blending Processes of rotor.Shown in two parametric results such as Fig. 1 (a) and Fig. 1 (b).
From Fig. 1 (a)：Counter balance torque value (7.59NM) in modified wood fibre -1/PP mixed processes is not less than
Modified wood fibre/PP values (4.03NM).This illustrates that the viscosity of modified wood fibre and the PP melts formed reduces
47%, the mobility of melt rises significantly；
In addition from Fig. 1 (b)：The energy released in modified wood fibre -1/PP process is generally lower than unmodified
Wood fibre/PP, this explanation is during machine-shaping, between modified wood fibre and material and machine barrel and rotor
Heat caused by friction is reduced.By further checking that sample is found：Modified fibre -1/PP samples do not find coking phenomenon.
Embodiment 2：
Step 1：The polyhexamethylene guanide phosphate solution of 25wt% is diluted to the aqueous solution of 5wt%, adds in hydroxide
Sodium solution, by its pH value adjustment to 11.5, labeled as solution A；By graphite oxide microplate, distilled water is added in, is kept for 80 DEG C, ultrasound
10min prepares the aqueous solution of 2.5wt%, adds in aqueous hydrochloric acid solution, is 3.8 by pH value adjustment, labeled as B solution.
Step 2：20g wood fibres are weighed, in the solution A of 100ml, ultrasound 15min at 80 DEG C, strainer filtering, 80 DEG C
Lower Quick-air-drying；In the B solution of 100ml, ultrasound 10min at 85 DEG C, strainer filtering, Quick-air-drying at 80 DEG C；It repeats above-mentioned
Operation 5 times is placed in 105 DEG C of baking oven dry 3h and obtains wood fibre, labeled as modified wood fibre -2.
The heat decomposition curve of wood fibre is analyzed with thermogravimetry, the starting of obtained modified wood fibre -2
Decomposition temperature is：168℃；Maximum decomposition temperature：375℃；(initial decomposition temperature of initial wood mass fiber is：159℃；It is maximum
Decomposition temperature：361℃).As it can be seen that the thermal stability of modified wood fibre -2 is better than initial wood mass fiber.
Due to torque rheometer, structure is similar, and material amounts are few with actual production equipment (mixer, extruder etc.), institute
The processes such as mixing, extrusion can be simulated in the lab, particularly suitable for optimization factory formula and process conditions.Haake torque rheology
The energy that instrument records reaction torque and release of the material to rotor or screw rod generation in mixed process changes with time, wherein
Counter balance torque value and material molten after melt viscosity and mobility it is corresponding.Counter balance torque value is lower, and material is being sheared
Under effect, viscosity when reaching melt stability is lower, and mobility during processing is better.
By wood fibre, polypropylene (PP) and maleic anhydride inoculated polypropylene with 20:75:5 weight percent,
170 DEG C, rotor speed 30rad/min, melt blending is carried out with Haake torque rheology instrument, is remembered automatically during melt blending
Record following parameter：The energy (E) released in the torque (M) and Blending Processes of rotor.Two parametric results such as Fig. 2 (a) and Fig. 2
(b) shown in.
From Fig. 2 (a)：Counter balance torque value (7.59NM) in modified wood fibre -2/PP mixed processes is not less than
Modified wood fibre/PP values (3.95NM).This illustrates the smaller drop of viscosity of modified wood fibre and the PP melts formed
Low 53%, the mobility of melt rises apparent.
In addition from Fig. 2 (b)：The energy released in modified wood fibre -1/PP process is generally lower than unmodified
Wood fibre/PP, this explanation is during machine-shaping, between modified wood fibre and material and machine barrel and rotor
Heat caused by friction is reduced.By further checking that sample is found：Modified fibre -2/PP samples do not find coking phenomenon.
Embodiment 3：
Step 1：The polyhexamethylene guanide phosphate solution of 25wt% is diluted to the aqueous solution of 5wt%, adds in hydroxide
Sodium solution, by its pH value adjustment to 11, labeled as solution A；By graphite oxide microplate, distilled water is added in, is kept for 60 DEG C, ultrasound
8min prepares the aqueous solution of 2.5wt%, adds in aqueous hydrochloric acid solution, is 3 by pH value adjustment, labeled as B solution.
Step 2：20g wood fibres are weighed, in the solution A of 100ml, ultrasound 12min at 75 DEG C, strainer filtering, 80 DEG C
Lower Quick-air-drying；In the B solution of 100ml, 5~10min of ultrasound at 80 DEG C, strainer filtering, Quick-air-drying at 80 DEG C；In repetition
Operation 5 times is stated, dry 2.5h is placed in 105 DEG C of baking oven and obtains wood fibre, labeled as modified wood fibre -3.
The heat decomposition curve of wood fibre is analyzed with thermogravimetry, the starting of obtained modified wood fibre -3
Decomposition temperature is：171℃；Maximum decomposition temperature：378℃；(initial decomposition temperature of initial wood mass fiber is：171℃；It is maximum
Decomposition temperature：361℃).As it can be seen that the thermal stability of modified wood fibre -3 is better than initial wood mass fiber.
Due to torque rheometer, structure is similar, and material amounts are few with actual production equipment (mixer, extruder etc.), institute
The processes such as mixing, extrusion can be simulated in the lab, particularly suitable for optimization factory formula and process conditions.Haake torque rheology
The energy that instrument records reaction torque and release of the material to rotor or screw rod generation in mixed process changes with time, wherein
Counter balance torque value and material molten after melt viscosity and mobility it is corresponding.Counter balance torque value is lower, and material is being sheared
Under effect, viscosity when reaching melt stability is lower, and mobility during processing is better.
By wood fibre, polypropylene (PP) and maleic anhydride inoculated polypropylene with 20:75:5 weight percent,
170 DEG C, rotor speed 30rad/min, melt blending is carried out with Haake torque rheology instrument, is remembered automatically during melt blending
Record following parameter：The energy (E) released in the torque (M) and Blending Processes of rotor.Two parametric results such as Fig. 3 (a) and Fig. 3
(b) shown in.
From Fig. 3 (a)：Counter balance torque value (7.59NM) in modified wood fibre -3/PP mixed processes is not less than
Modified wood fibre/PP values (3.65NM).This illustrates the smaller drop of viscosity of modified wood fibre and the PP melts formed
Low 52%, the mobility of melt rises apparent.
In addition from Fig. 3 (b)：The energy released in modified wood fibre -1/PP process is generally lower than unmodified
Wood fibre/PP, this explanation is during machine-shaping, between modified wood fibre and material and machine barrel and rotor
Heat caused by friction is reduced.By further checking that sample is found：Modified fibre -3/PP samples do not find coking phenomenon.
Embodiment 4：
Step 1：The polyhexamethylene guanide phosphate solution of 25wt% is diluted to the aqueous solution of 5wt%, adds in hydroxide
Sodium solution, by its pH value adjustment to 11, labeled as solution A；By graphite oxide microplate, distilled water is added in, is kept for 75 DEG C, ultrasound
8min prepares the aqueous solution of 2.5wt%, adds in aqueous hydrochloric acid solution, is 3.5 by pH value adjustment, labeled as B solution.
Step 2：20g wood fibres are weighed, in the solution A of 100ml, 10~15min of ultrasound at 78 DEG C, strainer filtering,
Quick-air-drying at 80 DEG C；In the B solution of 100ml, 5~10min of ultrasound at 82 DEG C, strainer filtering, Quick-air-drying at 80 DEG C；Weight
Aforesaid operations 5 times again are placed in 105 DEG C of baking oven dry 3h and obtain wood fibre, labeled as modified wood fibre -4.
The heat decomposition curve of wood fibre is analyzed with thermogravimetry, the starting of obtained modified wood fibre -4
Decomposition temperature is：169℃；Maximum decomposition temperature：385℃；(initial decomposition temperature of initial wood mass fiber is：159℃；It is maximum
Decomposition temperature：361℃).As it can be seen that the thermal stability of modified wood fibre -4 is better than initial wood mass fiber.
Due to torque rheometer, structure is similar, and material amounts are few with actual production equipment (mixer, extruder etc.), institute
The processes such as mixing, extrusion can be simulated in the lab, particularly suitable for optimization factory formula and process conditions.Haake torque rheology
The energy that instrument records reaction torque and release of the material to rotor or screw rod generation in mixed process changes with time, wherein
Counter balance torque value and material molten after melt viscosity and mobility it is corresponding.Counter balance torque value is lower, and material is being sheared
Under effect, viscosity when reaching melt stability is lower, and mobility during processing is better.
By wood fibre, polypropylene (PP) and maleic anhydride inoculated polypropylene with 20:75:5 weight percent,
170 DEG C, rotor speed 30rad/min, melt blending is carried out with Haake torque rheology instrument, is remembered automatically during melt blending
Record following parameter：The energy (E) released in the torque (M) and Blending Processes of rotor.Two parametric results such as Fig. 4 (a) and Fig. 4
(b) shown in.
From Fig. 4 (a)：Counter balance torque value (7.59NM) in modified wood fibre -4/PP mixed processes is not less than
Modified wood fibre/PP values (2.93NM).This illustrates the smaller drop of viscosity of modified wood fibre and the PP melts formed
Low 61%, the mobility of melt rises apparent.
In addition from Fig. 4 (b)：The energy released in modified wood fibre -1/PP process is generally lower than unmodified
Wood fibre/PP, this explanation is during machine-shaping, between modified wood fibre and material and machine barrel and rotor
Heat caused by friction is reduced.By further checking that sample is found：Modified fibre -4/PP samples do not find coking phenomenon.
Embodiment 5：
Step 1：The polyhexamethylene guanide phosphate solution of 25wt% is diluted to the aqueous solution of 5wt%, adds in hydroxide
Sodium solution, by its pH value adjustment to 11, labeled as solution A；By graphite oxide microplate, distilled water is added in, is kept for 65 DEG C, ultrasound
8min prepares the aqueous solution of 2.5wt%, adds in aqueous hydrochloric acid solution, is 3.2 by pH value adjustment, labeled as B solution.
Step 2：20g wood fibres are weighed, in the solution A of 100ml, 10~15min of ultrasound at 75 DEG C, strainer filtering,
Quick-air-drying at 80 DEG C；In the B solution of 100ml, 5~10min of ultrasound at 72 DEG C, strainer filtering, Quick-air-drying at 80 DEG C；Weight
Aforesaid operations 5 times again are placed in 105 DEG C of baking oven dry 2h and obtain wood fibre, labeled as modified wood fibre -5.
The heat decomposition curve of wood fibre is analyzed with thermogravimetry, the starting of obtained modified wood fibre -5
Decomposition temperature is：170℃；Maximum decomposition temperature：381℃；(initial decomposition temperature of initial wood mass fiber is：159℃；It is maximum
Decomposition temperature：361℃).As it can be seen that the thermal stability of modified wood fibre -5 is better than initial wood mass fiber.
Due to torque rheometer, structure is similar, and material amounts are few with actual production equipment (mixer, extruder etc.), institute
The processes such as mixing, extrusion can be simulated in the lab, particularly suitable for optimization factory formula and process conditions.Haake torque rheology
The energy that instrument records reaction torque and release of the material to rotor or screw rod generation in mixed process changes with time, wherein
Counter balance torque value and material molten after melt viscosity and mobility it is corresponding.Counter balance torque value is lower, and material is being sheared
Under effect, viscosity when reaching melt stability is lower, and mobility during processing is better.
By wood fibre, polypropylene (PP) and maleic anhydride inoculated polypropylene with 20:75:5 weight percent,
170 DEG C, rotor speed 30rad/min, melt blending is carried out with Haake torque rheology instrument, is remembered automatically during melt blending
Record following parameter：The energy (E) released in the torque (M) and Blending Processes of rotor.Two parametric results such as Fig. 4 (a) and Fig. 4
(b) shown in.
From Fig. 5 (a)：Counter balance torque value (7.59NM) in modified wood fibre -5/PP mixed processes is not less than
Modified wood fibre/PP values (2.87NM).This illustrates the smaller drop of viscosity of modified wood fibre and the PP melts formed
Low 62%, the mobility of melt rises apparent.
In addition from Fig. 5 (b)：The energy released in modified wood fibre -1/PP process is generally lower than unmodified
Wood fibre/PP, this explanation is during machine-shaping, between modified wood fibre and material and machine barrel and rotor
Heat caused by friction is reduced.By further checking that sample is found：Modified fibre -5/PP samples do not find coking phenomenon.
Claims (9)
1. a kind of preparation method for the wood fibre for optimizing wood plastic composite preparation process, it is characterised in that include following step
Suddenly：
Step 1：Solution A and B solution are prepared respectively；
Step 2：Wood fibre is weighed, air-dried after immersing solution A and B solution and carries out repeatedly, being finally dried to obtain modified wood
Matter fiber.
2. a kind of preparation method of wood fibre for optimizing wood plastic composite preparation process according to claim 1,
It is characterized in that：Prepared by the solution A in the step 1 is specially：Polyhexamethylene guanide phosphate solution is taken, adds in sodium hydroxide
Solution adjusts pH value, as solution A.
3. a kind of preparation method of wood fibre for optimizing wood plastic composite preparation process according to claim 2,
It is characterized in that：In the step 1, the polyhexamethylene guanide phosphate solution is contains 5wt% polyhexamethylene guanide phosphoric acid
The aqueous solution of salt.
4. a kind of preparation method of wood fibre for optimizing wood plastic composite preparation process according to claim 2,
It is characterized in that：The pH value of polyhexamethylene guanide phosphate solution is adjusted to 10.5~11.5 by the step 1 with sodium hydroxide.
5. a kind of preparation method of wood fibre for optimizing wood plastic composite preparation process according to claim 1,
It is characterized in that：Prepared by the B solution in the step 1 is specially：It is molten that graphite oxide microplate is added in into distilled water acquisition graphite oxide
Liquid is kept for 50~80 DEG C, 5~10min of ultrasound, is prepared and is obtained graphite oxide solution, is added in hydrochloric acid solution and is adjusted pH value, as B
Solution.
6. a kind of preparation method of wood fibre for optimizing wood plastic composite preparation process according to claim 5,
It is characterized in that：In the step 1, the graphite oxide solution is the aqueous solution containing 2.5wt% graphite oxides.
7. a kind of preparation method of wood fibre for optimizing wood plastic composite preparation process according to claim 5,
It is characterized in that：In the step 1, the pH value of polyhexamethylene guanide phosphate solution is adjusted to 2.7~3.8 with aqueous hydrochloric acid solution.
8. a kind of preparation method of wood fibre for optimizing wood plastic composite preparation process according to claim 5,
It is characterized in that：The step 2 is specially：
2.1) 20g wood fibres are weighed；
2.2) it immerses in the solution A of 100ml, 10~15min of ultrasound at 70~80 DEG C, strainer filtering, the quick wind at 80 DEG C
It is dry；It is immersed again in the B solution of 100ml after air-drying, 5~10min of ultrasound at 75~85 DEG C, strainer filtering, it is quick at 80 DEG C
It air-dries；
2.3) it repeats the above steps and 2.2) carries out 5 times, be subsequently placed in 105 DEG C of baking oven dry 2~3h and obtain wood fibre.
9. a kind of preparation method of the wood fibre of optimization wood plastic composite preparation process according to claim 1 or 8,
It is characterized in that：The length of the wood fibre (wood fibre before modified) of the step 2 be 1~8mm, a diameter of 10~
50um。
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106633977A (en) * | 2016-11-23 | 2017-05-10 | 浙江农林大学 | Nanometer matter/biomass fibrous composite and preparation method for nanometer matter/biomass fibrous composite |
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| CN107129630A (en) * | 2017-05-09 | 2017-09-05 | 泰山医学院 | A kind of conduction/Anti-static PP base wood-plastic composite material and preparation method thereof |
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| CN106633977A (en) * | 2016-11-23 | 2017-05-10 | 浙江农林大学 | Nanometer matter/biomass fibrous composite and preparation method for nanometer matter/biomass fibrous composite |
| CN106928738A (en) * | 2017-01-22 | 2017-07-07 | 浙江农林大学 | High temperature resistant grain hulls/polyolefin functional master batch and preparation method thereof |
| CN107129630A (en) * | 2017-05-09 | 2017-09-05 | 泰山医学院 | A kind of conduction/Anti-static PP base wood-plastic composite material and preparation method thereof |
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