CN106220820A - A kind of uniform dispersing method of lignocellulose - Google Patents

A kind of uniform dispersing method of lignocellulose Download PDF

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Publication number
CN106220820A
CN106220820A CN201610697960.7A CN201610697960A CN106220820A CN 106220820 A CN106220820 A CN 106220820A CN 201610697960 A CN201610697960 A CN 201610697960A CN 106220820 A CN106220820 A CN 106220820A
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processed material
lignocellulose
filtrated
filtrate
microwave
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谢裕梦
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72Polyisocyanates or polyisothiocyanates
    • C08G18/74Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/76Polyisocyanates or polyisothiocyanates cyclic aromatic
    • C08G18/7657Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
    • C08G18/7664Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
    • C08G18/7671Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/64Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63
    • C08G18/6492Lignin containing materials; Wood resins; Wood tars; Derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/6505Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen the low-molecular compounds being compounds of group C08G18/32 or polyamines of C08G18/38
    • C08G18/6511Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen the low-molecular compounds being compounds of group C08G18/32 or polyamines of C08G18/38 compounds of group C08G18/3203
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72Polyisocyanates or polyisothiocyanates
    • C08G18/73Polyisocyanates or polyisothiocyanates acyclic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72Polyisocyanates or polyisothiocyanates
    • C08G18/74Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/75Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
    • C08G18/758Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing two or more cycloaliphatic rings
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72Polyisocyanates or polyisothiocyanates
    • C08G18/74Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/76Polyisocyanates or polyisothiocyanates cyclic aromatic
    • C08G18/7614Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Polyurethanes Or Polyureas (AREA)

Abstract

The invention provides the uniform dispersing method of a kind of lignocellulose, belong to chemical field, including raw material pulverizing, alkali process, microwave acid treatment, polymerization process and regrinding.The lignocellulose processed by the present invention, it is processed by acid, alkali and makes powder body embrittlement, expands its microcellular structure, graft reaction is passed through with polymer, and combine physics process for refining, make the lignocellulose good dispersion made, fineness can reach 300~800 mesh, and can remain in that microcellular structure;Adding in coating, it can dispersed be opened so that coating have excellent insulation, heat insulation, insulate against sound, insulate and permeability, thermal expansion is not flaked, and improves anti-deep layer cracking performance and scraping and wiping resistance performance.

Description

A kind of uniform dispersing method of lignocellulose
Technical field
The invention belongs to chemical field, particularly relate to the uniform dispersing method of a kind of lignocellulose.
Background technology
Lignocellulose (lignocellulose) is that natural reproducible timber obtains through chemical treatment, Mechanical Method processing Organic wadding fibrous material, nontoxic, tasteless, pollution-free, "dead".Lignocellulose is water insoluble, weak acid and hydroxide Sodium solution;PH value is neutral, can improve system corrosion resistance;Its proportion is little, specific surface area is big, have excellent insulation, heat insulation, every Sound, insulation and permeability, thermal expansion is not the most flaked and is not ftractureed;Higher wet film intensity and coverage effect;Have excellent Pliability and dispersibility, form tridimensional network, enhance support force and the endurance of system, can improve system after mixing Stability, intensity, degree of compaction and the uniformity;The structural viscosity of wood fibre, the prefabricated slurry (dry and wet material) making to process equal Even property maintains the original state and stablizes and reduce contraction and the expansion of system, makes the precision of construction or prefabricated component be greatly improved;Have the strongest Antifreeze and solar heat protection ability.Therefore lignocellulose be widely used in water-proof putty powder, exterior-wall heat insulation slurry, mineral mortar, ceramic tile glue In knot agent and wall surface mortar.But the manufacture method of the lignocellulose of routine causes it to disperse not, affect the anti-deep of coating Layer cracking performance, reduces its scratch-resistant ability.
Summary of the invention
For solving above-mentioned technical problem, the invention provides the uniform dispersing method of a kind of lignocellulose.
The uniform dispersing method of a kind of lignocellulose, comprises the following steps:
1) raw material pulverizing, smashes into the coarse powder of 10~50 mesh by raw material;
2) alkali process, coarse powder is soaked in mass concentration be 5~10% sodium hydroxide solution in, temperature is 20~100 DEG C, soak 1~8h, being filtrated to get filtrate is processed material A;
3) microwave acid treatment, it is 5~the hydrochloric acid of 10%, 3~6% strongly acidic styrene that processed material A is placed in mass concentration Cation exchanger resin and 4~7% silicofluoric acid solution in, be then placed within 1000 watts, the microwave Muffle furnace of 2450MHz In, do dry type or wet type microwave combustion method, temperature is between 100~150 DEG C, and the process time is 1~5h, is filtrated to get filtrate For processed material B;
4) polymerization processes, by processed material B, diisocyanate, HMPA, alcohol compound according to 100:2~ The ratio mixing of 5:5~8:150~200, in the environment of 50~100 DEG C, stirring reflection 30~100min, is filtrated to get filtrate For processed material C;
5) regrinding, in processed material C, addition 0.05~0.1% grinding aid are ground, and screening obtains 300~800 Purpose fine powder.
Further, comprise the following steps:
1) raw material pulverizing, smashes into the coarse powder of 10~50 mesh by raw material;
2) alkali process, coarse powder is soaked in the sodium hydroxide solution that mass concentration is 8%, temperature is 80 DEG C, soak 1~ 8h, being filtrated to get filtrate is processed material A;
3) microwave acid treatment, is placed in hydrochloric acid, 4% strongly acidic styrene's cation that mass concentration is 7% by processed material A Exchanger resin and 5% silicofluoric acid solution in, be then placed within 1000 watts, in the microwave Muffle furnace of 2450MHz, do dry type or Wet type microwave combustion method, temperature is between 120 DEG C, and the process time is 3h, and being filtrated to get filtrate is processed material B;
4) polymerization processes, by processed material B, diisocyanate, HMPA, alcohol compound according to 100:3:7: The ratio mixing of 180, stirring reflection 70min in the environment of 50~100 DEG C, being filtrated to get filtrate is processed material C;
5) regrinding, adds 0.08% grinding aid in processed material C and is ground, and it is thin that screening obtains 300~800 purposes Powder.
Further, described diisocyanate is at least one in MDI, TDI, HDI, HMDI.
Further, described alcohol compound is at least in ethanol, ethylene glycol, propylene glycol, butanediol, hexanediol Kind.
Further, described grinding aid is organic-silicon-modified polyacrylate and the sodium silicate of equivalent.
The beneficial effects of the present invention is: the lignocellulose processed by the present invention, it is processed by acid, alkali and makes powder Body is brittle, expand its microcellular structure, with polymer by graft reaction, and combines physics process for refining so that making wooden Cellulose good dispersion, fineness can reach 300~800 mesh, and can remain in that microcellular structure;Adding in coating, it can Dispersed open so that coating have excellent insulation, heat insulation, insulate against sound, insulate and permeability, thermal expansion is not flaked, Improve anti-deep layer cracking performance and scraping and wiping resistance performance.
Detailed description of the invention
Technical scheme is described further below, but claimed scope is not limited to described.
Embodiment one
Present embodiments provide the uniform dispersing method of a kind of lignocellulose, comprise the following steps:
1) raw material pulverizing, smashes into the coarse powder of 10~50 mesh by raw material;
2) alkali processes, and is soaked in by coarse powder in the sodium hydroxide solution that mass concentration is 5%, and temperature is 20 DEG C, soaks 1h, Being filtrated to get filtrate is processed material A;
3) microwave acid treatment, is placed in hydrochloric acid, 3% strongly acidic styrene's cation that mass concentration is 5% by processed material A Exchanger resin and 4% silicofluoric acid solution in, be then placed within 1000 watts, in the microwave Muffle furnace of 2450MHz, do dry type or Wet type microwave combustion method, temperature is between 100 DEG C, and the process time is 1h, and being filtrated to get filtrate is processed material B;
4) polymerization processes, by processed material B, diisocyanate, HMPA, alcohol compound according to 100:2:5: The ratio mixing of 150, stirring reflection 30min in the environment of 50 DEG C, being filtrated to get filtrate is processed material C;Two described isocyanides Acid esters is at least one in MDI, TDI, HDI, HMDI, and the present embodiment selects MDI, and described alcohol compound is ethanol, second At least one in glycol, propylene glycol, butanediol, hexanediol, the present embodiment selects ethanol;
5) regrinding, adds 0.05% grinding aid in processed material C and is ground, and it is thin that screening obtains 300~800 purposes Powder, described grinding aid is organic-silicon-modified polyacrylate and the sodium silicate of equivalent.
Embodiment two
Present embodiments provide the uniform dispersing method of a kind of lignocellulose, comprise the following steps:
1) raw material pulverizing, smashes into the coarse powder of 10~50 mesh by raw material;
2) alkali processes, and is soaked in by coarse powder in the sodium hydroxide solution that mass concentration is 10%, and temperature is 100 DEG C, soaks 8h, being filtrated to get filtrate is processed material A;
3) microwave acid treatment, processed material A is placed in hydrochloric acid that mass concentration is 10%, 6% strongly acidic styrene be sun from Sub-exchange resin and 4~7% silicofluoric acid solution in, be then placed within 1000 watts, in the microwave Muffle furnace of 2450MHz, do dry Formula or wet type microwave combustion method, temperature is between 150 DEG C, and the process time is 5h, and being filtrated to get filtrate is processed material B;
4) polymerization processes, by processed material B, diisocyanate, HMPA, alcohol compound according to 100:5:8: The ratio mixing of 200, stirring reflection 100min in the environment of 100 DEG C, being filtrated to get filtrate is processed material C;Described two are different Cyanate is at least one in MDI, TDI, HDI, HMDI, and the present embodiment selects HDI;Described alcohol compound be ethanol, At least one in ethylene glycol, propylene glycol, butanediol, hexanediol, the present embodiment selects butanediol;
5) regrinding, adds 0.1% grinding aid in processed material C and is ground, and it is thin that screening obtains 300~800 purposes Powder, described grinding aid is organic-silicon-modified polyacrylate and the sodium silicate of equivalent.
Embodiment three
Present embodiments provide the uniform dispersing method of a kind of lignocellulose, comprise the following steps:
1) raw material pulverizing, smashes into the coarse powder of 10~50 mesh by raw material;
2) alkali process, coarse powder is soaked in the sodium hydroxide solution that mass concentration is 8%, temperature is 80 DEG C, soak 1~ 8h, being filtrated to get filtrate is processed material A;
3) microwave acid treatment, is placed in hydrochloric acid, 4% strongly acidic styrene's cation that mass concentration is 7% by processed material A Exchanger resin and 5% silicofluoric acid solution in, be then placed within 1000 watts, in the microwave Muffle furnace of 2450MHz, do dry type or Wet type microwave combustion method, temperature is between 120 DEG C, and the process time is 3h, and being filtrated to get filtrate is processed material B;
4) polymerization processes, by processed material B, diisocyanate, HMPA, alcohol compound according to 100:3:7: The ratio mixing of 180, stirring reflection 70min in the environment of 50~100 DEG C, being filtrated to get filtrate is processed material C;Described two Isocyanates is at least one in MDI, TDI, HDI, HMDI, and the present embodiment selects MDI and HMDI of equivalent;Described alcohols Compound is at least one in ethanol, ethylene glycol, propylene glycol, butanediol, hexanediol, and the present embodiment selects the ethylene glycol of equivalent And propylene glycol;
5) regrinding, adds 0.08% grinding aid in processed material C and is ground, and it is thin that screening obtains 300~800 purposes Powder;Described grinding aid is organic-silicon-modified polyacrylate and the sodium silicate of equivalent.

Claims (5)

1. the uniform dispersing method of a lignocellulose, it is characterised in that: comprise the following steps:
1) raw material pulverizing, smashes into the coarse powder of 10~50 mesh by raw material;
2) alkali process, coarse powder is soaked in mass concentration be 5~10% sodium hydroxide solution in, temperature is 20~100 DEG C, leaching Bubble 1~8h, being filtrated to get filtrate is processed material A;
3) microwave acid treatment, processed material A is placed in mass concentration be 5~the hydrochloric acid of 10%, 3~6% strongly acidic styrene be sun Ion exchange resin and 4~7% silicofluoric acid solution in, be then placed within 1000 watts, in the microwave Muffle furnace of 2450MHz, do Dry type or wet type microwave combustion method, temperature is between 100~150 DEG C, and the process time is 1~5h, is filtrated to get filtrate for place Reason thing B;
4) polymerization processes, by processed material B, diisocyanate, HMPA, alcohol compound according to 100:2~5:5~ The ratio mixing of 8:150~200, stirring reflection 30~100min in the environment of 50~100 DEG C, it is filtrated to get filtrate for processing Thing C;
5) regrinding, in processed material C, addition 0.05~0.1% grinding aid are ground, and screening obtains 300~800 purposes Fine powder.
2. the uniform dispersing method of lignocellulose as claimed in claim 1, it is characterised in that: comprise the following steps:
1) raw material pulverizing, smashes into the coarse powder of 10~50 mesh by raw material;
2) alkali processes, and is soaked in by coarse powder in the sodium hydroxide solution that mass concentration is 8%, and temperature is 80 DEG C, soaks 1~8h, Being filtrated to get filtrate is processed material A;
3) microwave acid treatment, is placed in hydrochloric acid, 4% strongly acidic styrene's cation exchange that mass concentration is 7% by processed material A Resin and 5% silicofluoric acid solution in, be then placed within 1000 watts, in the microwave Muffle furnace of 2450MHz, do dry type or wet type Microwave combustion method, temperature is between 120 DEG C, and the process time is 3h, and being filtrated to get filtrate is processed material B;
4) polymerization processes, by processed material B, diisocyanate, HMPA, alcohol compound according to 100:3:7:180 Ratio mixing, in the environment of 50~100 DEG C stirring reflection 70min, being filtrated to get filtrate is processed material C;
5) regrinding, adds 0.08% grinding aid in processed material C and is ground, and screening obtains the fine powder of 300~800 mesh i.e. Can.
3. the uniform dispersing method of lignocellulose as claimed in claim 1 or 2, it is characterised in that: two described Carbimide .s Ester is at least one in MDI, TDI, HDI, HMDI.
4. the uniform dispersing method of lignocellulose as claimed in claim 1, it is characterised in that: described alcohol compound is At least one in ethanol, ethylene glycol, propylene glycol, butanediol, hexanediol.
5. the uniform dispersing method of lignocellulose as claimed in claim 1, it is characterised in that: described grinding aid is equivalent Organic-silicon-modified polyacrylate and sodium silicate.
CN201610697960.7A 2016-08-20 2016-08-20 A kind of uniform dispersing method of lignocellulose Pending CN106220820A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10501588B2 (en) * 2015-08-18 2019-12-10 Jiangnan University Grafting method for rice straw fiber modification

Citations (3)

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Publication number Priority date Publication date Assignee Title
CN101481459A (en) * 2008-12-23 2009-07-15 中国人民解放军总后勤部军需装备研究所 Micropore ligno-cellulose ultramicro powder, as well as preparation method and application thereof
CN101638442A (en) * 2009-08-28 2010-02-03 中国科学院西双版纳热带植物园 Method for hydrolyzing lignocellulose
CN105377958A (en) * 2013-05-03 2016-03-02 威尔迪亚公司 Production methodology of hydrolyzed collagen using swiftlet nest as raw material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101481459A (en) * 2008-12-23 2009-07-15 中国人民解放军总后勤部军需装备研究所 Micropore ligno-cellulose ultramicro powder, as well as preparation method and application thereof
CN101638442A (en) * 2009-08-28 2010-02-03 中国科学院西双版纳热带植物园 Method for hydrolyzing lignocellulose
CN105377958A (en) * 2013-05-03 2016-03-02 威尔迪亚公司 Production methodology of hydrolyzed collagen using swiftlet nest as raw material

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* Cited by examiner, † Cited by third party
Title
李子东等: "《胶粘剂助剂》", 30 June 2009 *
郑水林等: "《非金属矿加工技术与应用手册》", 30 May 2005 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10501588B2 (en) * 2015-08-18 2019-12-10 Jiangnan University Grafting method for rice straw fiber modification

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Address after: 541000 Guilin, the Guangxi Zhuang Autonomous Region, Yanshan District, zhe Mu town 091 County Road North 250 meters green square village

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Address before: 541000 Guilin, the Guangxi Zhuang Autonomous Region City, county, Longshui Town, Shan Po village, Tao Tian La village 018

Applicant before: Xie Yumeng

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Application publication date: 20161214