CN102276848B - Method for modifying and pretreating bacterium mushroom stick used for preparing wood-plastic composite material - Google Patents
Method for modifying and pretreating bacterium mushroom stick used for preparing wood-plastic composite material Download PDFInfo
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- CN102276848B CN102276848B CN201110211935A CN201110211935A CN102276848B CN 102276848 B CN102276848 B CN 102276848B CN 201110211935 A CN201110211935 A CN 201110211935A CN 201110211935 A CN201110211935 A CN 201110211935A CN 102276848 B CN102276848 B CN 102276848B
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- bacterium mushroom
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Abstract
The invention relates to a method for modifying and pretreating a bacterium mushroom stick used for preparing a wood-plastic composite material, and the method comprises the following steps of: (1) firstly crushing, stoving and screening the bacterium mushroom stick; and (2) then carrying out chemical graft modification: stirring the bacterium mushroom stick subjected to the crushing, stoving and screening at high speed; when the temperature reaches 105-115 DEG C, adding a chemical initiator monomer, then adding a coupling agent, and continuing stirring at high speed; and when the temperature reaches 120-125 DEG C, stopping the stirring, wherein the following raw materials are adopted in parts by weight: 90-120 parts of the bacterium mushroom stick subjected to the crushing, stoving and screening, 0.1-1 part of the chemical initiator monomer and 0.5-4 parts of the coupling agent. According to the invention, waste material can be changed into things of value, the bacterium mushroom stick can be well combined with PVC (poly vinyl chloride) resin to prepare a wood fiber raw material of the wood-plastic composite material, thus environmental pollution problem caused by the bacterium mushroom stick is solved and production cost is reduced.
Description
Technical field
The present invention relates to the modification pretreatment process that a kind of bacterium mushroom rod is used for the wood plastic composite preparation.
Background technology
Bacterium mushroom rod is that agricultural planting is produced the left next waste of becteriums product.A large amount of bacterium mushroom rods are deposited in around the mushroom plantation, rural area, are difficult to dispose, and the time has been grown and also can send a kind of septic taste, contaminate environment.Need use a large amount of lignocellulose raw materials in the preparation process of wood plastic composite, but find through the mass analysis that the sample of bacterium mushroom rod is done: the staple of bacterium mushroom rod differs very big with the staple of making the needed lignocellulose raw material of wood plastic composite: the lignocellulose molecular weight in the bacterium mushroom rod raw material significantly reduces, the content of other organic composition also reduces in a large number, molecular weight reduces.Therefore, if bacterium mushroom rod directly uses, adds in PVC wood plastic composite and the goods, will directly reduce the physical and mechanical properties of wood plastic composite.
Summary of the invention
In order to solve existing in prior technology the problems referred to above; The invention provides the modification pretreatment process that a kind of bacterium mushroom rod is used for the wood plastic composite preparation; It can be turned waste into wealth; Make bacterium mushroom rod become can with the lignocellulose raw material of polyvinyl chloride resin good combination with the preparation wood plastic composite, both solved the problem of environmental pollution that bacterium mushroom rod is caused, reduced production cost again.
Technical scheme of the present invention is to constitute like this, and a kind of bacterium mushroom rod is used for the modification pretreatment process of wood plastic composite preparation, and it is characterized in that: it may further comprise the steps:
1. carry out fragmentation, oven dry and the Screening Treatment of bacterium mushroom rod earlier, the moisture content of bacterium mushroom rod is remained in 8%, remove impurity through screening through oven dry;
2. then carrying out grafting modification handles: the bacterium mushroom rod high-speed stirring that will pass through fragmentation, oven dry and Screening Treatment earlier; When temperature reaches 105-115 ℃, add the chemical initiator monomer, make its molecule chain end form reactive group at bacterium mushroom rod wood fibre; Then add coupling agent, continue high-speed stirring; , temperature stops to stir when reaching 120-125 ℃; In this step, the weight proportion of each raw material is following:
Bacterium mushroom rod 90-120 part through fragmentation, oven dry and Screening Treatment;
1 part of chemical initiator monomer 0.1-;
4 parts of coupling agent 0.5-.
Said chemical initiator monomer is made up of Di Cumyl Peroxide 99 or maleic anhydride, and said coupling agent is made up of titanate coupling agent or silane coupling agent or aluminate coupling agent.
Coupling agent is multi-functional organic cpds, an end solubilized or be diffused in the polyvinyl chloride resin of interface region, and the other end can form key with hydrophilic radical in the wood fibre combine the interfacial adhesion between raising filler and matrix.As a result, one side direct graft polymerization between the part molecule of bacterium mushroom rod raw material forms crosslinked; On the other hand, the polyfunctional group of coupling agent can make wood fibre and polyvinyl chloride resin merge well, forms an organic whole, thereby improves the physical and mechanical properties of wood plastic composite.
Compared to prior art; The present invention has following remarkable advantage: the present invention is through handling the modification preplasticizing of bacterium mushroom rod; The refuse of this agriculture prodn of bacterium mushroom rod is turned waste into wealth; Make bacterium mushroom rod become can with the lignocellulose raw material of polyvinyl chloride resin good combination with the preparation wood plastic composite, both solved the problem of environmental pollution that bacterium mushroom rod is caused, reduced production cost again.In addition,, therefore both enlarged raw-material optional scope, also played the effect of practicing thrift timber resources because lignocellulose raw materials such as the alternative after treatment wood powder that generally uses at present of bacterium mushroom rod, bamboo powder are produced qualified Wood Plastics Composite Product.
Embodiment
Below in conjunction with embodiment and embodiment content of the present invention is elaborated:
The specific embodiment of the invention relates to the modification pretreatment process that a kind of bacterium mushroom rod is used for the wood plastic composite preparation, and it is characterized in that: it may further comprise the steps:
1. carry out fragmentation, oven dry and the Screening Treatment of bacterium mushroom rod earlier, the moisture content of bacterium mushroom rod is remained in 8%, remove impurity through screening through oven dry;
2. then carrying out grafting modification handles: the bacterium mushroom rod high-speed stirring that will pass through fragmentation, oven dry and Screening Treatment earlier; When temperature reaches 105-115 ℃, add chemical initiator monomer (can constitute) by Di Cumyl Peroxide 99 or maleic anhydride, make its molecule chain end form reactive group at bacterium mushroom rod wood fibre; Then add coupling agent (can constitute), continue high-speed stirring by titanate coupling agent or silane coupling agent; , temperature stops to stir when reaching 120-125 ℃; In this step, the weight proportion of each raw material is following:
Bacterium mushroom rod 90-120 part through fragmentation, oven dry and Screening Treatment;
1 part of chemical initiator monomer 0.1-;
4 parts of coupling agent 0.5-.
Above step is removed moisture too much in the wood fibre mainly by the frictional heat of high-speed stirring; And the high-shear of stirring by height accomplishes wood fibre carried out sufficient chemical modification, eliminates the polarity of wood fibre as much as possible.
In addition, the present invention provides also that will to pass through the pretreated bacterium mushroom of modification rod following with the preparation method that polyvinyl chloride resin and various auxiliary agent are mixed with wood plastic composite:
(1) high speed blend: polyvinyl chloride resin, pretreated wood fibre and the various auxiliary agent of modification are carried out preplasticizing through the high-speed stirring blend; Described auxiliary agent comprises lubricant, thermo-stabilizer, anti-impact modifier and whipping agent, and the concrete grammar of high speed blend is following:
1. earlier with polyvinyl chloride resin and thermo-stabilizer high-speed stirring mixing together;
2. when temperature reaches 75-90 ℃, Yi Bian add lubricant, anti-impact modifier and through the pretreated wood fibre of modification, Yi Bian continue high-speed stirring;
3. when temperature reaches 110-116 ℃, Yi Bian add whipping agent, Yi Bian continue high-speed stirring;
4. when temperature reaches 118-125 ℃, stop to stir, material is transferred to cooling vessel is cooled to below 60 ℃, for use.
In addition, as required, in the 3. stage in above-mentioned steps, when adding whipping agent, also can add an amount of mould inhibitor and/or UV stabilizer.If wood plastic composite is used for the open air, then preferably add UV stabilizer, add if be used for indoor then do not need.The interpolation of mould inhibitor is mainly decided according to the degree of drying of environment for use.
(time and temperature requirement) is most important the order of addition(of ingredients) of each raw material and reinforced opportunity in this step, directly has influence on the quality of product.Said polyvinyl chloride resin, lubricant, thermo-stabilizer, anti-impact modifier, whipping agent, mould inhibitor, UV stabilizer and following through the weight proportion between the bacterium mushroom rod of fragmentation, oven dry and Screening Treatment:
Polyvinyl chloride resin: 100 parts,
Bacterium mushroom rod through fragmentation, oven dry and Screening Treatment: 90-120 part,
Lubricant: 2-4 part,
Thermo-stabilizer: 6-10 part,
Anti-impact modifier: 8-12 part,
Whipping agent: 1-3 part,
Mould inhibitor: 0.5-1 part,
UV stabilizer: 0.5-1 part.
Available starting material are following in the wood plastic composite:
Said polyvinyl chloride resin comprises SG5 or SG7;
Said lubricant comprises at least a in paraffin or the stearate; Because the mobile extreme difference of wood fibre adds the flowability that lubricant can strengthen wood fibre, increases the flowability of polyvinyl chloride resin simultaneously, keeps any surface finish of wood plastic product.
Said thermo-stabilizer comprises calcium-zinc composite stabilizing agent, organotin stabilizer, rare-earth stabilizer or lead salt one package stabilizer;
Said anti-impact modifier comprises at least a among thermoplastic elastic body C PE (chlorinatedpolyethylene) or the ACR (propenoate); Anti-impact modifier can strengthen wood plastic composite shock resistance, improve material snappiness, improve the resistance to low temperature of material;
Said whipping agent comprises heat release type whipping agent and endothermic blowing agent;
Said mould inhibitor comprises nano composite antibiotic material, and said nano composite antibiotic material comprises at least a in nano titanium oxide or the sterilant; The purpose that adds mould inhibitor is to prevent that wood plastic composite from going mouldy, and it can prevent the growth of flavus, black mold etc. effectively;
Said UV stabilizer comprises the UV-531 one package stabilizer.UV stabilizer can reduce and prevent and treat the destruction of ultraviolet ray to wood plastic composite effectively, prolongs the duration of service and the life-span of product.
(2) extrusion moulding: the mass transport that preplasticizing is good fully plastifies material to forcing machine under the proper temperature condition, will plastify good material afterwards and clamp-on in the forming mould, under the effect of squeeze, makes the material extrusion moulding; Making material carry out abundant plastifying proper temperature condition is 170-200 ℃;
(3) cooling and shaping: with the parison cools typing of extrusion moulding.The method of described cooling and shaping is successively through cooling die and cooling bath cooling and shaping with the parison of extrusion moulding.
In addition, in the preprocessing process of bacterium mushroom rod, as required, also can an amount of mineral filler be added in the bacterium mushroom rod, make bacterium mushroom rod with an amount of mineral filler high-speed stirring; Perhaps at the 2. described adding lubricant of stage, anti-impact modifier and in the pretreated bacterium mushroom rod, add an amount of mineral filler high-speed stirring together of step (1) through modification; Said mineral filler comprises CaCO
3Or at least a in the talcum powder; The weight proportion of the bacterium mushroom rod of said mineral filler and process fragmentation, oven dry and Screening Treatment is: mineral filler 0-20 part, and through the excellent 90-120 part of the bacterium mushroom of fragmentation, oven dry and Screening Treatment.Certainly, in the actual production process, the interpolation of mineral filler is not essential.
The described auxiliary agent of step (1) also can comprise auxiliary addition agent; Said auxiliary addition agent comprises at least a in epoxy soybean oil, DOP, static inhibitor or the pigment; The interpolation time of said auxiliary addition agent is the 2. stage in step (1), adds high-speed stirring with lubricant, anti-impact modifier with through pretreated bacterium mushroom rod; The weight proportion of said polyvinyl chloride resin and auxiliary addition agent is following: 100 parts of polyvinyl chloride resins: auxiliary addition agent 5-8 part.The interpolation of auxiliary addition agent also is dispensable, mainly decides according to the actual performance needs of the wood plastic composite of producing.
Embodiment 1
1. carry out fragmentation, oven dry and the Screening Treatment of bacterium mushroom rod earlier, the moisture content of bacterium mushroom rod is remained in 8%, remove impurity through screening through oven dry;
2. then carrying out grafting modification handles: the bacterium mushroom rod 90kg high-speed stirring that will pass through fragmentation, oven dry and Screening Treatment earlier; When temperature reaches 105 ℃, add Di Cumyl Peroxide 99 0.1kg, make its molecule chain end form reactive group at bacterium mushroom rod wood fibre; Then add titanate coupling agent 0.5kg, continue high-speed stirring; , temperature stops to stir when reaching about 120 ℃, and for use.
Embodiment 2
1. carry out fragmentation, oven dry and the Screening Treatment of bacterium mushroom rod earlier, the moisture content of bacterium mushroom rod is remained in 8%, remove impurity through screening through oven dry;
2. then carrying out grafting modification handles: the bacterium mushroom rod 105kg high-speed stirring that will pass through fragmentation, oven dry and Screening Treatment earlier; When temperature reaches 110 ℃, add Di Cumyl Peroxide 99 0.5kg, make its molecule chain end form reactive group at bacterium mushroom rod wood fibre; Then add titanate coupling agent 2kg, continue high-speed stirring; , temperature stops to stir when reaching about 122 ℃, and for use.
Embodiment 3
1. carry out fragmentation, oven dry and the Screening Treatment of bacterium mushroom rod earlier, the moisture content of bacterium mushroom rod is remained in 8%, remove impurity through screening through oven dry;
2. then carrying out grafting modification handles: the bacterium mushroom rod 120kg high-speed stirring that will pass through fragmentation, oven dry and Screening Treatment earlier; When temperature reaches 115 ℃, add Di Cumyl Peroxide 99 1kg, make its molecule chain end form reactive group at bacterium mushroom rod wood fibre; Then add titanate coupling agent 4kg, continue high-speed stirring; , temperature stops to stir when reaching about 125 ℃, and for use.
Embodiment 4
To pass through the pretreated bacterium mushroom rod of embodiment 1-3 modification and 100kg polyvinyl chloride resin, 3kg lubricant (employing paraffin), 8kg thermo-stabilizer (employing calcium-zinc composite stabilizing agent), 10kg anti-impact modifier (adopting CPE), 2kg whipping agent, 0.8kg mould inhibitor (employing nano titanium oxide) and 0.8kg UV stabilizer, and be mixed with according to following steps and obtain three groups of wood plastic composites (routine 4-1, routine 4-2, routine 4-3).
(1) high speed blend:
1. earlier with polyvinyl chloride resin and thermo-stabilizer high-speed stirring mixing together;
2. when temperature reaches 82 ℃, Yi Bian add lubricant, anti-impact modifier and through pretreated wood fibre, Yi Bian continue high-speed stirring;
3. when temperature reaches 112 ℃, Yi Bian add whipping agent, mould inhibitor and UV stabilizer, Yi Bian continue high-speed stirring;
4. when temperature reaches 120 ℃, stop to stir, material is transferred to cooling vessel is cooled to below 60 ℃, for use.
(3) extrusion moulding: the mass transport that preplasticizing is good fully plastifies material to forcing machine under 185 ℃ temperature condition, will plastify good material afterwards and clamp-on in the forming mould, under the effect of squeeze, makes the material extrusion moulding;
(4) cooling and shaping: the parison of extrusion moulding is passed through cooling die and cooling bath cooling and shaping successively.
Embodiment 5 (control group)
With other raw material of not enumerating, and prepare according to embodiment 4 listed steps through the pretreated bacterium mushroom of modification rod 100kg and embodiment 4.
The preparation effect comparison
One group of wood plastic composite that three groups of wood plastic composites that prepare through embodiment 4 and embodiment 5 prepare detects contrast as follows
In addition; Change the Di Cumyl Peroxide 99 among routine 4-1, routine 4-2, the routine 4-3 into maleic anhydride, change titanate coupling agent into silane coupling agent, all the other proportioning raw materials are identical with process step; The detected result basically identical of detected result and routine 4-1, routine 4-2, routine 4-3, positive and negative deviation is within 5%.
Claims (2)
1. modification pretreatment process that is used to prepare the bacterium mushroom rod of wood plastic composite, it is characterized in that: it may further comprise the steps:
1. carry out fragmentation, oven dry and the Screening Treatment of bacterium mushroom rod earlier, the moisture content of bacterium mushroom rod is remained in 8%, remove impurity through screening through oven dry;
2. then carrying out grafting modification handles: the bacterium mushroom rod high-speed stirring that will pass through fragmentation, oven dry and Screening Treatment earlier; When temperature reaches 105-115 ℃, add the chemical initiator monomer, make its molecule chain end form reactive group at bacterium mushroom rod wood fibre; Then add coupling agent, continue high-speed stirring; , temperature stops to stir when reaching 120-125 ℃; In this step, the weight proportion of each raw material is following:
Bacterium mushroom rod 90-120 part through fragmentation, oven dry and Screening Treatment;
Chemical initiator monomer 0.1-1 part;
Coupling agent 0.5-4 part;
Said chemical initiator monomer is made up of Di Cumyl Peroxide 99 or maleic anhydride.
2. the modification pretreatment process that is used to prepare the bacterium mushroom rod of wood plastic composite according to claim 1 is characterized in that: said coupling agent is made up of titanate coupling agent or silane coupling agent or aluminate coupling agent.
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| CN201110211935A CN102276848B (en) | 2011-07-27 | 2011-07-27 | Method for modifying and pretreating bacterium mushroom stick used for preparing wood-plastic composite material |
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| CN102276848B true CN102276848B (en) | 2012-09-26 |
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| CN103214751B (en) * | 2012-09-21 | 2015-06-17 | 上海工程技术大学 | PVC/agricultural waste composite material, and preparation method and application thereof |
| CN105985658A (en) * | 2015-02-15 | 2016-10-05 | 承德华鑫实业有限公司 | Composite material prepared from mushroom stick wastes and used for degradable flower pots, and molding method thereof |
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