CN105315936A - Preparing method for phenolic resin adhesive for wood - Google Patents
Preparing method for phenolic resin adhesive for wood Download PDFInfo
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- CN105315936A CN105315936A CN201510817033.XA CN201510817033A CN105315936A CN 105315936 A CN105315936 A CN 105315936A CN 201510817033 A CN201510817033 A CN 201510817033A CN 105315936 A CN105315936 A CN 105315936A
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Abstract
The invention provides a preparing method for phenolic resin adhesive for wood. The preparing method includes the following steps that 1, boron carbide powder is added into absolute ethyl alcohol after being dried and stirred to obtain mixed liquid, the mixed liquid is added into an ethyl alcohol solution of KH570, the mixed solution is stirred for reacting after the ph value is adjusted and then stands at the room temperature, and drying is carried out after suction filtration to obtain modified boron carbide for use; 2, by weight, 100 parts of phenol and 70-80 parts of a formaldehyde solution are added into a stirring kettle and uniformly stirred, then 10-15 parts of composite catalysts are added, after heating, a reaction is carried out at the constant temperature under stirring, 2-7 parts of an acid catalyst is added into the stirring kettle, a reaction continues to be carried out at the constant temperature under stirring, 9-10 parts of polyarylester and 5-6 parts of the modified boron carbide are added into the stirring kettle, and a reaction continues to be carried out at the constant temperature under stirring; 3, after the reaction is stopped, the product stands, is placed in deionized water to be washed, and is dehydrated through reduced pressure distillation, dehydration is stopped when the temperature rises to 105 DEG C, and the phenolic resin adhesive for wood is obtained after the product is naturally cooled to the room temperature. The adhesive prepared through the method is good in abrasive resistance, heat resistance and flame retardancy.
Description
Technical field:
The present invention relates to a kind of tackiness agent, particularly relate to a kind of preparation method of timber synvaren.
Background technology:
Resol, phenolicresin, is called for short PF.Resol is the general designation that phenols and aldehydes form resin under catalyst action, and phenols is phenol, cresols, xylenol, Resorcinol etc. mainly, aldehydes mainly formaldehyde, oxalic dialdehyde, furfural etc.Within 1872, first Germanization scholar Baeyer has synthesized resol, Belgian descendants American Bake orchid in 1907 proposes resol and to be heating and curing method, resol is made to realize suitability for industrialized production, within 1910, Berlin, Germany builds up the factory of the first in the world man novolak resin, has started the epoch of mankind's synthetic macromolecular compound.The kind of phenol, aldehyde, catalyzer classification, phenol produce diversified resol from the different of mol ratio of aldehyde, comprising: lacquer resins, heat-reactive phenolic resin and soluble phenolic resin, water soluble phenol resin.Solid phenolic resin is yellow, transparent, amorphous cake mass, and because being blush containing free phenol, proportion 1.25 ~ 1.30, is soluble in alcohol, water insoluble, stablizes water, weak acid, weak caustic solution.Liquid phenolic resin is yellow, dark brown liquid.In wood processing field, resol uses one of main glue kind widely, and its consumption is only second to urea-formaldehyde resin, and in especially water-fast in production, weathering resistance woodwork, resol has special meaning.
Such as, the Chinese patent that publication number is CN101870856B, publication date is 2012.07.18, application people is Yakeshi Tuofu Forestry Chemical Products Co., Ltd. discloses " bark powder phenolic-resin adhesive and preparation method thereof ", it adopts the base catalysis system comprising calcium sulfite to carry out activation treatment to tree bark powder, and the product Substitute For Partial phenol then using tree bark powder activation treatment to obtain is prepared from.The timber bark powder phenolic-resin adhesive viscosity of this invention is 200 ~ 2000mPa.s, solids content is 40 ~ 50%, wherein the alternative amount of phenol is 35 ~ 55%, and it has, and quality is good, low price, working condition requirement is low, catalytic erosion is little and can utilize the advantages such as existing glue production unit.But, there is certain defect in this tackiness agent: wear resistance is poor, simultaneously thermotolerance and flame retardant resistance not ideal enough.
Summary of the invention:
The technical problem to be solved in the present invention is to provide a kind of preparation method of timber synvaren, and the tackiness agent prepared has good wear resistance, thermotolerance and flame retardant resistance.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A preparation method for timber synvaren, its step is as follows:
(1) add in dehydrated alcohol by after boron carbide powder drying, mixed solution is obtained after stirring 30 parts of clocks, mixed solution is added in the ethanolic soln of KH570, ph value is regulated to be 5 stirring reaction at latter 90 DEG C 4 hours, left at room temperature 24 hours, suction filtration to be placed in the vacuum drying oven of 110 DEG C dry 24 hours, obtains modified carbonize boron for subsequent use;
(2) count by weight, 100 parts of phenol, 70-80 part formaldehyde solution are added stirring tank, 10-15 part composite catalyst is added after stirring, constant temperature stirring reaction 3 hours after being heated to 100 DEG C, 2-7 part an acidic catalyst is added stirring tank, continue constant temperature stirring reaction 2 hours, the modified carbonize boron that 9-10 part polyarylester and 5-6 part step (1) obtain is added stirring tank, continue constant temperature stirring reaction 5 hours;
(3) reaction leaves standstill 5 hours after stopping, and deionized water product being placed in 80 DEG C washs 5 times, and underpressure distillation is dewatered, and stops, obtaining timber phenolic resin adhesive after naturally cooling to room temperature when temperature rises to 105 DEG C.
Preferably, in step of the present invention (1), the purity of boron carbide powder is 90%.
Preferably, in step of the present invention (1), the massfraction of the ethanolic soln of KH570 is 70%.
Preferably, in step of the present invention (1), the weight ratio of boron carbide powder and KH570 is 20:1.
Preferably, in step of the present invention (1), stirring velocity is 1400r/min.
Preferably, in step of the present invention (2), the mass-dispersion of formaldehyde solution is 36%.
Preferably, in step of the present invention (2), composite catalyst is the mixture of acetic acid and copper sulfate.
Preferably, in step of the present invention (2), an acidic catalyst is phosphoric acid.
Preferably, in step of the present invention (2), the stirring velocity of stirring tank is 800r/min.
Preferably, in step of the present invention (3), vacuum tightness during underpressure distillation dehydration is 66mmHg.
Compared with prior art, the present invention has following beneficial effect:
(1) norbide another name black diamond, molecular formula is B4C, that (other two kinds is diamond to one of known three kinds of the hardest materials, cubic boron nitride), therefore there is splendid wear resistance, but its surface is wetting ability, and the consistency between oil loving phenolic resin as matrix resin is poor, thus the present invention carries out modification by silane coupling agent KH570 to it, the alkoxy portion hydrolysis of KH570 becomes silicone hydroxyl, with the boric acid of boron carbide powder remained on surface or the hydroxyl generation bonding reaction of absorption, the mutual polycondensation of silicone hydroxyl simultaneously between KH570, coupling agent coating film is defined on the surface of boron carbide powder, the wetting ability on norbide surface is become lipophilicity, improve the consistency between itself and resol, improve interface bond strength between the two, norbide can play isolation dual face in the base and bear the effect of most of frrction load, thus greatly reduce the wearing and tearing that are subject to of phenolic resin as matrix resin, significantly improve the wear resistance of sizing agent, in addition, the fusing point of norbide is very high, and thermotolerance and flame retardant resistance very well, therefore also effectively can improve thermotolerance and the flame retardant resistance of sizing agent.
(2) phenyl ring containing comparatively dense in the molecular structure of polyarylester, thus there is good thermotolerance, it is self-extingushing plastic simultaneously, there is higher oxygen index and flame retardant resistance, therefore formed with resol interface blended preferably after, can further improve thermotolerance and the flame retardant resistance of sizing agent.
Embodiment:
Describe the present invention in detail below in conjunction with specific embodiment, be used for explaining the present invention in this illustrative examples of the present invention and explanation, but not as a limitation of the invention.
Embodiment 1
The preparation method of timber synvaren, its step is as follows:
(1) by purity be 90% boron carbide powder drying after add in dehydrated alcohol, mixed solution is obtained after stirring 30 parts of clocks, mixed solution being added massfraction is in the ethanolic soln of the KH570 of 70%, the weight ratio of boron carbide powder and KH570 is 20:1, to regulate ph value to be 5 stirring velocitys at latter 90 DEG C to be under 1400r/min stirring reaction 4 hours, left at room temperature 24 hours, suction filtration to be placed in the vacuum drying oven of 110 DEG C dry 24 hours, obtains modified carbonize boron for subsequent use;
(2) count by weight, by 100 parts of phenol, 74 parts of mass-dispersion be 36% formaldehyde solution add stirring tank, 12 parts of composite catalysts are added after stirring---the mixture of acetic acid and copper sulfate, constant temperature stirring reaction 3 hours after being heated to 100 DEG C, by 2 parts of an acidic catalysts---phosphoric acid adds stirring tank, continue constant temperature stirring reaction 2 hours, the modified carbonize boron that 9.6 parts of polyarylesters and 6 parts of steps (1) obtain is added stirring tank, continue constant temperature stirring reaction 5 hours, the stirring velocity of stirring tank is 800r/min;
(3) reaction leaves standstill 5 hours after stopping, and deionized water product being placed in 80 DEG C washs 5 times, and vacuum tightness is underpressure distillation dehydration under 66mmHg, stops, obtaining timber phenolic resin adhesive after naturally cooling to room temperature when temperature rises to 105 DEG C.
Embodiment 2
The preparation method of timber synvaren, its step is as follows:
(1) by purity be 90% boron carbide powder drying after add in dehydrated alcohol, mixed solution is obtained after stirring 30 parts of clocks, mixed solution being added massfraction is in the ethanolic soln of the KH570 of 70%, the weight ratio of boron carbide powder and KH570 is 20:1, to regulate ph value to be 5 stirring velocitys at latter 90 DEG C to be under 1400r/min stirring reaction 4 hours, left at room temperature 24 hours, suction filtration to be placed in the vacuum drying oven of 110 DEG C dry 24 hours, obtains modified carbonize boron for subsequent use;
(2) count by weight, by 100 parts of phenol, 75 parts of mass-dispersion be 36% formaldehyde solution add stirring tank, 11 parts of composite catalysts are added after stirring---the mixture of acetic acid and copper sulfate, constant temperature stirring reaction 3 hours after being heated to 100 DEG C, by 7 parts of an acidic catalysts---phosphoric acid adds stirring tank, continue constant temperature stirring reaction 2 hours, the modified carbonize boron that 9.9 parts of polyarylesters and 5 parts of steps (1) obtain is added stirring tank, continue constant temperature stirring reaction 5 hours, the stirring velocity of stirring tank is 800r/min;
(3) reaction leaves standstill 5 hours after stopping, and deionized water product being placed in 80 DEG C washs 5 times, and vacuum tightness is underpressure distillation dehydration under 66mmHg, stops, obtaining timber phenolic resin adhesive after naturally cooling to room temperature when temperature rises to 105 DEG C.
Embodiment 3
The preparation method of timber synvaren, its step is as follows:
(1) by purity be 90% boron carbide powder drying after add in dehydrated alcohol, mixed solution is obtained after stirring 30 parts of clocks, mixed solution being added massfraction is in the ethanolic soln of the KH570 of 70%, the weight ratio of boron carbide powder and KH570 is 20:1, to regulate ph value to be 5 stirring velocitys at latter 90 DEG C to be under 1400r/min stirring reaction 4 hours, left at room temperature 24 hours, suction filtration to be placed in the vacuum drying oven of 110 DEG C dry 24 hours, obtains modified carbonize boron for subsequent use;
(2) count by weight, by 100 parts of phenol, 70 parts of mass-dispersion be 36% formaldehyde solution add stirring tank, 15 parts of composite catalysts are added after stirring---the mixture of acetic acid and copper sulfate, constant temperature stirring reaction 3 hours after being heated to 100 DEG C, by 5 parts of an acidic catalysts---phosphoric acid adds stirring tank, continue constant temperature stirring reaction 2 hours, the modified carbonize boron that 9.1 parts of polyarylesters and 5.4 parts of steps (1) obtain is added stirring tank, continue constant temperature stirring reaction 5 hours, the stirring velocity of stirring tank is 800r/min;
(3) reaction leaves standstill 5 hours after stopping, and deionized water product being placed in 80 DEG C washs 5 times, and vacuum tightness is underpressure distillation dehydration under 66mmHg, stops, obtaining timber phenolic resin adhesive after naturally cooling to room temperature when temperature rises to 105 DEG C.
Embodiment 4
The preparation method of timber synvaren, its step is as follows:
(1) by purity be 90% boron carbide powder drying after add in dehydrated alcohol, mixed solution is obtained after stirring 30 parts of clocks, mixed solution being added massfraction is in the ethanolic soln of the KH570 of 70%, the weight ratio of boron carbide powder and KH570 is 20:1, to regulate ph value to be 5 stirring velocitys at latter 90 DEG C to be under 1400r/min stirring reaction 4 hours, left at room temperature 24 hours, suction filtration to be placed in the vacuum drying oven of 110 DEG C dry 24 hours, obtains modified carbonize boron for subsequent use;
(2) count by weight, by 100 parts of phenol, 80 parts of mass-dispersion be 36% formaldehyde solution add stirring tank, 10 parts of composite catalysts are added after stirring---the mixture of acetic acid and copper sulfate, constant temperature stirring reaction 3 hours after being heated to 100 DEG C, by 6 parts of an acidic catalysts---phosphoric acid adds stirring tank, continue constant temperature stirring reaction 2 hours, the modified carbonize boron that 9.3 parts of polyarylesters and 5.1 parts of steps (1) obtain is added stirring tank, continue constant temperature stirring reaction 5 hours, the stirring velocity of stirring tank is 800r/min;
(3) reaction leaves standstill 5 hours after stopping, and deionized water product being placed in 80 DEG C washs 5 times, and vacuum tightness is underpressure distillation dehydration under 66mmHg, stops, obtaining timber phenolic resin adhesive after naturally cooling to room temperature when temperature rises to 105 DEG C.
Embodiment 5
The preparation method of timber synvaren, its step is as follows:
(1) by purity be 90% boron carbide powder drying after add in dehydrated alcohol, mixed solution is obtained after stirring 30 parts of clocks, mixed solution being added massfraction is in the ethanolic soln of the KH570 of 70%, the weight ratio of boron carbide powder and KH570 is 20:1, to regulate ph value to be 5 stirring velocitys at latter 90 DEG C to be under 1400r/min stirring reaction 4 hours, left at room temperature 24 hours, suction filtration to be placed in the vacuum drying oven of 110 DEG C dry 24 hours, obtains modified carbonize boron for subsequent use;
(2) count by weight, by 100 parts of phenol, 72 parts of mass-dispersion be 36% formaldehyde solution add stirring tank, 13 parts of composite catalysts are added after stirring---the mixture of acetic acid and copper sulfate, constant temperature stirring reaction 3 hours after being heated to 100 DEG C, by 4 parts of an acidic catalysts---phosphoric acid adds stirring tank, continue constant temperature stirring reaction 2 hours, the modified carbonize boron that 9 parts of polyarylesters and 5.5 parts of steps (1) obtain is added stirring tank, continue constant temperature stirring reaction 5 hours, the stirring velocity of stirring tank is 800r/min;
(3) reaction leaves standstill 5 hours after stopping, and deionized water product being placed in 80 DEG C washs 5 times, and vacuum tightness is underpressure distillation dehydration under 66mmHg, stops, obtaining timber phenolic resin adhesive after naturally cooling to room temperature when temperature rises to 105 DEG C.
Embodiment 6
The preparation method of timber synvaren, its step is as follows:
(1) by purity be 90% boron carbide powder drying after add in dehydrated alcohol, mixed solution is obtained after stirring 30 parts of clocks, mixed solution being added massfraction is in the ethanolic soln of the KH570 of 70%, the weight ratio of boron carbide powder and KH570 is 20:1, to regulate ph value to be 5 stirring velocitys at latter 90 DEG C to be under 1400r/min stirring reaction 4 hours, left at room temperature 24 hours, suction filtration to be placed in the vacuum drying oven of 110 DEG C dry 24 hours, obtains modified carbonize boron for subsequent use;
(2) count by weight, by 100 parts of phenol, 76 parts of mass-dispersion be 36% formaldehyde solution add stirring tank, 14 parts of composite catalysts are added after stirring---the mixture of acetic acid and copper sulfate, constant temperature stirring reaction 3 hours after being heated to 100 DEG C, by 3 parts of an acidic catalysts---phosphoric acid adds stirring tank, continue constant temperature stirring reaction 2 hours, the modified carbonize boron that 10 parts of polyarylesters and 5.7 parts of steps (1) obtain is added stirring tank, continue constant temperature stirring reaction 5 hours, the stirring velocity of stirring tank is 800r/min;
(3) reaction leaves standstill 5 hours after stopping, and deionized water product being placed in 80 DEG C washs 5 times, and vacuum tightness is underpressure distillation dehydration under 66mmHg, stops, obtaining timber phenolic resin adhesive after naturally cooling to room temperature when temperature rises to 105 DEG C.
After tested, the wear resistance of the tackiness agent that embodiment 1-6 obtains and comparative example, thermotolerance and flame retardant resistance are as shown in the table, wherein,
The Chinese patent of comparative example to be publication number be CN101870856B;
The annulus that wearability test adopts No. 45 steel to make and each sizing agent glued membrane were to mill 5 hours, and positive pressure is set to 20kg, and adopt wear testing machine quality measurement wear rate, quality wear rate is lower, shows that wear resistance is better;
Thermotolerance test process is, each sizing agent glued membrane is warming up to 150 DEG C with the speed of 20 DEG C/min, constant temperature 2 minutes, normal temperature is cooled to the speed of 20 DEG C/min, constant temperature 2 minutes, then be warming up to 500 DEG C with the speed of 20 DEG C/min, test the mass loss rate of each sizing agent glued membrane 350 DEG C time, mass loss rate is lower, shows that thermotolerance is better;
The oxygen index of each sizing agent is tested in flame retardant resistance test according to GB/T2406-2008, oxygen index is higher, shows that flame retardant resistance is better.
As seen from the above table, the quality wear rate of the tackiness agent that embodiment of the present invention 1-6 obtains, mass loss rate are all starkly lower than comparative example, and oxygen index is then all higher than comparative example, and wear resistance, thermotolerance, flame retardant resistance are all better.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (10)
1. a preparation method for timber synvaren, is characterized in that: its step is as follows:
(1) add in dehydrated alcohol by after boron carbide powder drying, mixed solution is obtained after stirring 30 parts of clocks, mixed solution is added in the ethanolic soln of KH570, ph value is regulated to be 5 stirring reaction at latter 90 DEG C 4 hours, left at room temperature 24 hours, suction filtration to be placed in the vacuum drying oven of 110 DEG C dry 24 hours, obtains modified carbonize boron for subsequent use;
(2) count by weight, 100 parts of phenol, 70-80 part formaldehyde solution are added stirring tank, 10-15 part composite catalyst is added after stirring, constant temperature stirring reaction 3 hours after being heated to 100 DEG C, 2-7 part an acidic catalyst is added stirring tank, continue constant temperature stirring reaction 2 hours, the modified carbonize boron that 9-10 part polyarylester and 5-6 part step (1) obtain is added stirring tank, continue constant temperature stirring reaction 5 hours;
(3) reaction leaves standstill 5 hours after stopping, and deionized water product being placed in 80 DEG C washs 5 times, and underpressure distillation is dewatered, and stops, obtaining timber phenolic resin adhesive after naturally cooling to room temperature when temperature rises to 105 DEG C.
2. the preparation method of a kind of timber synvaren according to claim 1, is characterized in that: in described step (1), the purity of boron carbide powder is 90%.
3. the preparation method of a kind of timber synvaren according to claim 1, is characterized in that: in described step (1), the massfraction of the ethanolic soln of KH570 is 70%.
4. the preparation method of a kind of timber synvaren according to claim 1, is characterized in that: in described step (1), the weight ratio of boron carbide powder and KH570 is 20:1.
5. the preparation method of a kind of timber synvaren according to claim 1, it is characterized in that: in described step (1), stirring velocity is 1400r/min.
6. the preparation method of a kind of timber synvaren according to claim 1, is characterized in that: in described step (2), the mass-dispersion of formaldehyde solution is 36%.
7. the preparation method of a kind of timber synvaren according to claim 1, it is characterized in that: in described step (2), composite catalyst is the mixture of acetic acid and copper sulfate.
8. the preparation method of a kind of timber synvaren according to claim 1, it is characterized in that: in described step (2), an acidic catalyst is phosphoric acid.
9. the preparation method of a kind of timber synvaren according to claim 1, is characterized in that: in described step (2), the stirring velocity of stirring tank is 800r/min.
10. the preparation method of a kind of timber synvaren according to claim 1, is characterized in that: in described step (3), and vacuum tightness during underpressure distillation dehydration is 66mmHg.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105904526A (en) * | 2016-06-28 | 2016-08-31 | 南京林业大学 | Manufacturing method of high-corrosion-resistance reconstructing material for outdoor use |
CN106590488A (en) * | 2016-12-21 | 2017-04-26 | 怀宁县凉亭建材有限责任公司 | Method for preparing oxidized lignin phenolic resin adhesive |
CN111944331A (en) * | 2020-08-04 | 2020-11-17 | 上海核工程研究设计院有限公司 | Surface modification treatment method of anti-settling boron carbide powder |
Citations (3)
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CN102399522A (en) * | 2011-10-09 | 2012-04-04 | 中国科学院化学研究所 | Organic / inorganic composite adhesive |
CN102627927A (en) * | 2012-03-26 | 2012-08-08 | 黑龙江省科学院石油化学研究院 | Medium temperature curing high temperature resistant phenolic adhesive |
CN104449499A (en) * | 2014-11-13 | 2015-03-25 | 山东永泰化工有限公司 | Phenolic resin adhesive and preparation method thereof |
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2015
- 2015-11-23 CN CN201510817033.XA patent/CN105315936B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102399522A (en) * | 2011-10-09 | 2012-04-04 | 中国科学院化学研究所 | Organic / inorganic composite adhesive |
CN102627927A (en) * | 2012-03-26 | 2012-08-08 | 黑龙江省科学院石油化学研究院 | Medium temperature curing high temperature resistant phenolic adhesive |
CN104449499A (en) * | 2014-11-13 | 2015-03-25 | 山东永泰化工有限公司 | Phenolic resin adhesive and preparation method thereof |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105904526A (en) * | 2016-06-28 | 2016-08-31 | 南京林业大学 | Manufacturing method of high-corrosion-resistance reconstructing material for outdoor use |
CN106590488A (en) * | 2016-12-21 | 2017-04-26 | 怀宁县凉亭建材有限责任公司 | Method for preparing oxidized lignin phenolic resin adhesive |
CN111944331A (en) * | 2020-08-04 | 2020-11-17 | 上海核工程研究设计院有限公司 | Surface modification treatment method of anti-settling boron carbide powder |
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