CN104212123A - Composite alkaline phenolic resin curing agent, preparation method and application - Google Patents
Composite alkaline phenolic resin curing agent, preparation method and application Download PDFInfo
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- CN104212123A CN104212123A CN201410442679.XA CN201410442679A CN104212123A CN 104212123 A CN104212123 A CN 104212123A CN 201410442679 A CN201410442679 A CN 201410442679A CN 104212123 A CN104212123 A CN 104212123A
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Abstract
The invention discloses a composite alkaline phenolic resin curing agent, a preparation method and an application, belonging to the technical field of curing of phenolic resin. The curing agent comprises a polyhydroxymethyl urea mixture, carbonate, organic ester compounds, polyvinyl alcohol and water. The preparation method comprises the following steps: sequentially putting the polyhydroxymethyl urea mixture, water and carbonate into a reactor; uniformly stirring; adding polyvinyl alcohol and the organic ester compounds; and uniformly stirring to obtain the composite alkaline phenolic resin curing agent. The curing agent is high in curing speed, excellent in curing performance and long in service life. The preparation method is simple and convenient to operate.
Description
Technical field
The present invention relates to a kind of compound alkalescent phenol resin solidifying agent, preparation method and application, belong to the technical field of phenolic resin curing.
Background technology
Alkalescent phenol resin is to carry out a kind of high molecular polymer prepared by polycondensation by formaldehyde and phenol according to certain mol ratio under alkaline condition, mainly for the manufacture of various plastics, coating, tackiness agent, synthon, fire-retardant material etc.Resol has high, the resistance to boiling water of Joint strength, the advantage such as heat-resisting as tackiness agent, is widely used in the manufacture of outdoor structure wood-based plate.The curing of resol is the process that linear soluble resin is changed into tridimensional network, is the continuation of polycondensation, is the critical process that forms bonding strength, and the bonding quality of wood-based panel product is played to vital effect.Alkalescent phenol resin is 130～140 DEG C in temperature, do not add under the condition of solidifying agent, can realize curing.But compared with the urea-formaldehyde resin adhesive conventional with wood-based plate, phenolic resin curing speed is slow, set time that need to be longer while fully solidifying, as while suppressing glued board, hot pressing time is about 70s/mm, than the hot pressing time of urea-formaldehyde resin (55s/mm) many 21% left and right.Thereby, in production must extend hot pressing time, guarantee quality product, affected wood-based panel product production efficiency, cause energy and devices consume larger, these have all limited resol widespread use in Wood-based Panel Production as tackiness agent.For this reason, need supporting development alkalescent phenol resin quick curing agent, promote alkalescent phenol resin fast setting, make it have the wood-based plate hot pressing time close or even shorter with conventional urea-formaldehyde resin, under the prerequisite that does not increase any raw materials cost, enhance productivity beyond doubt, increase product profit.
Current alkalescent phenol resin quick curing agent is mainly to adopt single component solidifying agent, as sodium carbonate, ethyl acetate, methyl-formiate, Phenylsulfonic acid, formic acid, hexamethylenetetramine etc., although these solidifying agent can improve the curing speed of alkalescent phenol resin, also can affect usability and the manufacturability of resol in the time of manufacture product simultaneously.For example, resol, as adhesive of artificial board needs more than 4 hours working life in the time preparing glued board, adds after solidifying agent, and the viscosity of resol changed very little in 3～5 hours.But, while being dissolved in resol normal temperature due to single-component solidifying agent, can discharge hydrogen ion, cause it that gelatin phenomenon occurs very soon, cause the working life of resol shorter (less than 2 hours), require lower than Wood-based Panel Production more than 4 hours, thereby application in the Wood-based Panel Production that is unsuitable for preparing at resol.Therefore, need to develop a efficiently, solidifying agent that can rapid curing phenolic resin during for unreactiveness, high temperature under normal temperature, and do not affect the working life of resin and the bonding strength of glueing joint glued board thereof.
The domestic patent about alkalescent phenol resin solidifying agent only has several sections, as disclosed a kind of solidifying agent at a slow speed of the alkalescent phenol resin for large-scale steel-casting production and application in the publication number patent of invention document that is CN101343382A, it is mainly the curing speed of resin of slowing down.Application publication number is to disclose for the curing solidifying agent of alkalescent phenol resin in winter in the patent of invention document of CN101823120A, solves the problem of phenolic resin curing difficulty in winter.From existing patent, be not also used for up to now the suitable composite curing agent of rapid curing phenolic resin.
Summary of the invention
Add for existing solidifying agent that the resol causing after resol shortens working life, bonding strength reduces, the unconspicuous shortcoming of curing speed facilitation effect to, one of object of invention is to provide a kind of composite phenol formaldehyde resin quick curing agent, described solidifying agent curing speed is fast, curing performance is excellent, and working life is long; Two of object is to provide a kind of preparation method of composite phenol formaldehyde resin curing agent, and described method is simple to operate, can give full play to the promoter action that the each component of solidifying agent strengthens the raising of phenolic resin curing speed, prolongation working life, bonding strength.
The object of the invention is to be achieved through the following technical solutions.
A kind of composite phenol formaldehyde resin quick curing agent, described solidifying agent comprises many methylolureas mixture, carbonate, organic esters, polyethylene alcohol and water, taking solidifying agent total mass as 100%, each component and quality percentage composition are as follows:
The preparation method of many methylolureas mixture is as follows:
Urea and formaldehyde are reacted to 2～2.5h at 85～90 DEG C, obtain described many methylolureas mixture;
Wherein, preferably 1.2～1.5:1 of the mol ratio of urea and formaldehyde;
One or both in the preferred sodium carbonate of carbonate and salt of wormwood;
More than one in organic esters ethyl acetate, propylene carbonate, glycerol acetate and methyl-formiate;
A preparation method for composite phenol formaldehyde resin curing agent, described method concrete steps are as follows:
Successively many methylolureas mixture, water and carbonate are put in reactor, stirred, add polyvinyl alcohol and organic esters, stir 15～30min, obtain described composite phenol formaldehyde tree solidifying agent.
A kind of composite phenol formaldehyde resin curing agent is applied to solidifying of resol, and wherein, described resol is that solid content is 40～50%, and apparent viscosity is the heat-reactive phenolic resin of 150～1500 centipoises;
Preferably 2～5:100 of the mass ratio of solidifying agent and resol when application.
Beneficial effect
(1) after solidifying agent of the present invention directly being added in alkalescent phenol resin and evenly mixing, can effectively improve the curing speed of resol, reduce the hot pressing time of the glued board of preparation, thereby improved the production efficiency of plywood product;
(2) solidifying agent of the present invention contains many methylolureas mixture, at ambient temperature, many methylolureas mixture is very stable, can suppress the release of sodium carbonate or salt of wormwood, organic esters middle acid substance, there is good shock absorption, so can greatly extend the working life of resol;
(3) sodium carbonate in solidifying agent of the present invention or salt of wormwood, organic esters are under hot pressing temperature effect, decomposite carbanion, middle strong acid, the two collaborative fast setting that promotes resol, simultaneously many methylols of many methylolureas mixture also can with active room in resol or methylol generation cross-linking polymerization, thereby improve the bonding strength that resol glueds joint glued board;
(4) solidifying agent of the present invention adds in alkalescent phenol resin and can fully solidify alkalescent phenol resin, make its fast setting, also can improve the bonding strength that alkalescent phenol resin glueds joint glued board simultaneously, and the alkalescent phenol resin after interpolation solidifying agent has longer working life, can adapt to the requirement of production operation of artificial boards;
(5) preparation method of solidifying agent of the present invention is simple, easy and simple to handle.
Embodiment
With specific embodiment in detail the present invention is described in detail below, but is not limited to this.
The main agents information of mentioning in following examples is in table 1; Key instrument and facility information are in table 2.
Table 1
Table 2
Embodiment 1
A kind of composite phenol formaldehyde resin quick curing agent, taking described solidifying agent total mass as 100%, each component and quality percentage composition are as follows:
A preparation method for composite phenol formaldehyde resin curing agent, described method concrete steps are as follows:
(1) be to react 2.5h under 90 DEG C of conditions by 1.2 mole of urea and 1 moles of formaldehyde in temperature, obtain many methylolureas mixture;
(2) many methylolureas of 50kg mixture, 20kg water and 15kg sodium carbonate are put into batch can in order, stir, add 10kg polyvinyl alcohol and 5kg ethyl acetate mix and blend 15min, obtain solidifying agent of the present invention.
The key technical indexes of gained solidifying agent is: solids content is that 55%, pH is 9.2, and density is 1.04, storage period >=30 day.
Embodiment 2
A kind of composite phenol formaldehyde resin quick curing agent, taking described solidifying agent total mass as 100%, each component and quality percentage composition are as follows:
A preparation method for composite phenol formaldehyde resin curing agent, described method concrete steps are as follows:
(1) be to react 2h under 90 DEG C of conditions by 1.5 mole of urea and 1 moles of formaldehyde in temperature, obtain many methylolureas mixture;
(2) many methylolureas of 70kg mixture, 10kg water and 15kg salt of wormwood are put into batch can in order, stir, add 4kg polyvinyl alcohol and 1kg ethyl acetate mix and blend 30min, obtain solidifying agent of the present invention.
The key technical indexes of gained solidifying agent is: solids content is that 63%, pH is 10.1, and density is 1.15, storage period >=30 day.
Embodiment 3
A kind of composite phenol formaldehyde resin quick curing agent, taking described solidifying agent total mass as 100%, each component and quality percentage composition are as follows:
A preparation method for composite phenol formaldehyde resin curing agent, described method concrete steps are as follows:
(1) be to react 2.3h under 87 DEG C of conditions by 1.3 mole of urea and 1 moles of formaldehyde in temperature, obtain many methylolureas mixture;
(2) many methylolureas of 60kg mixture, 10kg water and 25kg salt of wormwood are put into batch can in order, stir, add 2kg polyvinyl alcohol and 3kg propylene carbonate mix and blend 20min, obtain solidifying agent of the present invention.
The key technical indexes of gained solidifying agent is: solids content is that 58%, pH is 8.6, and density is 1.13, storage period >=30 day.
Embodiment 4
A kind of composite phenol formaldehyde resin quick curing agent, taking described solidifying agent total mass as 100%, each component and quality percentage composition are as follows:
A preparation method for composite phenol formaldehyde resin curing agent, described method concrete steps are as follows:
(1) be to react 2.5h under 87 DEG C of conditions by 1.3 mole of urea and 1 moles of formaldehyde in temperature, obtain many methylolureas mixture;
(2) many methylolureas of 55kg mixture, 15kg water, 5kg salt of wormwood and 15kg sodium carbonate are put into batch can in order, stir, add 7kg polyvinyl alcohol and 3kg methyl-formiate mix and blend 25min, obtain solidifying agent of the present invention.
The key technical indexes of gained solidifying agent is: solids content 61%, pH9.2, density 1.14, storage period >=30 day.
Embodiment 5
A kind of composite phenol formaldehyde resin quick curing agent, taking described solidifying agent total mass as 100%, each component and quality percentage composition are as follows:
A preparation method for composite phenol formaldehyde resin curing agent, described method concrete steps are as follows:
(1) be to react 2h under 90 DEG C of conditions by 1.2 mole of urea and 1 moles of formaldehyde in temperature, obtain many methylolureas mixture;
(2) many methylolureas of 60kg mixture, 20kg water and 10kg sodium carbonate are put into batch can in order, stir, add 6kg polyvinyl alcohol and 4kg glycerol acetate mix and blend 20min, obtain solidifying agent of the present invention.
The key technical indexes of gained solidifying agent is: solids content is that 57%, pH is 8.9, and density is 1.07, storage period >=30 day.
Embodiment 6
A kind of composite phenol formaldehyde resin quick curing agent, taking described solidifying agent total mass as 100%, each component and quality percentage composition are as follows:
A preparation method for composite phenol formaldehyde resin curing agent, described method concrete steps are as follows:
(1) be to react 2.5h under 85 DEG C of conditions by 1.2 mole of urea and 1 moles of formaldehyde in temperature, obtain many methylolureas mixture;
(2) many methylolureas of 60kg mixture, 12kg water and 18kg salt of wormwood are put into batch can in order, stir, add 5kg polyvinyl alcohol, 3kg ethyl acetate and 2kg methyl-formiate mix and blend 15min, obtain solidifying agent of the present invention.
The key technical indexes of gained solidifying agent is: solids content is that 60%, pH is 9.6, and density is 1.11, storage period >=30 day.
Embodiment 7
A kind of composite phenol formaldehyde resin quick curing agent, taking described solidifying agent total mass as 100%, each component and quality percentage composition are as follows:
A preparation method for composite phenol formaldehyde resin curing agent, described method concrete steps are as follows:
(1) be to react 2.3h under 90 DEG C of conditions by 1.4 mole of urea and 1 moles of formaldehyde in temperature, obtain many methylolureas mixture;
(2) many methylolureas of 65kg mixture, 10kg water, 10kg sodium carbonate and 10kg salt of wormwood are put into batch can in order, stir, add 2kg polyvinyl alcohol, 2kg ethyl acetate and 1kg propylene carbonate mix and blend 30min, obtain solidifying agent of the present invention.
The key technical indexes of gained solidifying agent is: solids content is that 65%, pH is 10.5, and density is 1.17, storage period >=30 day.
Embodiment 8
A kind of composite phenol formaldehyde resin quick curing agent, taking described solidifying agent total mass as 100%, each component and quality percentage composition are as follows:
A preparation method for composite phenol formaldehyde resin curing agent, described method concrete steps are as follows:
(1) be to react 2h under 90 DEG C of conditions by 1.5 mole of urea and 1 moles of formaldehyde in temperature, obtain many methylolureas mixture;
(2) many methylolureas of 50kg mixture, 10kg water, 5kg sodium carbonate and 20kg salt of wormwood are put into batch can in order, stir, add 10kg polyvinyl alcohol, 2kg ethyl acetate, 2kg propylene carbonate and 1kg glycerol acetate mix and blend 25min, obtain solidifying agent of the present invention.
The key technical indexes of gained solidifying agent is: solids content is that 58%, pH is 9.5, and density is 1.09, storage period >=30 day.
Embodiment 9
Utilize the effect of following evidence composite phenol formaldehyde resin curing agent of the present invention in resol application, particular content is as follows:
First,, by solidifying agent prepared specific embodiment 1-8, be numbered respectively sample 1, sample 2, sample 3, sample 4, sample 5, sample 6, sample 7 and sample 8.Then by sample 1, sample 2, sample 3, sample 4, sample 5, sample 6, sample 7 and sample 8 are according to 2:100, 2:100, 3:100, 3:100, 4:100, 4:100, 5:100, the mass ratio of 5:100 respectively with resol 1 (solid content is 40%, and apparent viscosity is 1500 centipoises), resol 2 (solid content is 45%, and apparent viscosity is 150 centipoises), resol 3 (solid content is 50%, and apparent viscosity is 680 centipoises), resol 4 (solid content is 48%, and apparent viscosity is 500 centipoises), resol 5 (solid content is 50%, and apparent viscosity is 800 centipoises), resol 6 (solid content is 42%, and apparent viscosity is 500 centipoises), resol 7 (solid content is 45%, and apparent viscosity is 300 centipoises), resol 8 (solid content is 48%, and apparent viscosity is 750 centipoises) mixes, and obtains respectively tackiness agent 1, tackiness agent 2, tackiness agent 3, tackiness agent 4, tackiness agent 5, tackiness agent 6, tackiness agent 7 and tackiness agent 8.To not add the resol 1 tackiness agent A in contrast of solidifying agent simultaneously, add the resol 1 tackiness agent B in contrast of sodium carbonate, wherein, the quality of sodium carbonate is resol 1 weight 2%.Respectively prepared tackiness agent 1, tackiness agent 2, tackiness agent 3, tackiness agent 4, tackiness agent 5, tackiness agent 6, tackiness agent 7, tackiness agent 8 and contrast tackiness agent A, contrast tackiness agent B are cured to velocity test, detection working life and 5 layers of poplar plywoods preparation.
Wherein, the test of curing speed and working life is carried out according to the corresponding method of detection of regulation in GB/T14074-2006 " wood adhesive and the resin method of inspection thereof ", and the probe temperature of curing speed is 130 DEG C, and test result is as shown in table 1.
Prepare in 5 layers of plywood process, add the flour of tackiness agent weight 20% when impregnation, veneer is 5 years quick growth poplar wood veneers (400 millimeters of length, 400 millimeters of width, 1.7 millimeters of thickness), water ratio 12%; The heat pressing process of 5 layers of glued board is: 1.0Mpa, and temperature is 130 DEG C, the time is 3.5 minutes.
According to the bonding strength of 8 kinds of tackiness agent of type Ⅰ plywood bonding strength testing method test of regulation in GB/T17657-1999 " test methods of evaluating the properties of wood-based panels and surface decorated wood-based panels " and the prepared 5 layers of glued board of 2 contrast tackiness agent, result is as shown in table 2.
Table 1
Table 2
As can be seen from Table 1, solidifying agent of the present invention adds the prepared tackiness agent 1-8 of resol to, than contrast tackiness agent A-B, its curing speed significantly increases, improve resol and prepared the production efficiency of wood-base fibre and particle panel material product, saved cost of labor, increased the profit of wood-based panel product; Compare with contrasting tackiness agent 2, significantly increase working life of resol of adding solidifying agent of the present invention, all more than 5 hours, meets resol as the tackiness agent requirement of needs more than 4 hours working life in the time preparing wood-based plate.
The glued board that adds the production of adhesive of solidifying agent of the present invention has higher bonding strength, meet type Ⅰ plywood national standard (being not less than 0.70MPa), and the bonding strength of contrast production of adhesive glued board is lower than 0.70MPa, do not reach type Ⅰ plywood national standard.
Wherein, resol 1-8 is heat-reactive phenolic resin, purchased from Tai Er chemical industry (Beijing) company limited.
The present invention includes but be not limited to above embodiment, every any being equal to of carrying out under the principle of spirit of the present invention, replaces or local improvement, all will be considered as within protection scope of the present invention.
Claims (7)
1. a compound alkalescent phenol resin solidifying agent, is characterized in that: taking solidifying agent total mass as 100%, each component and quality percentage composition are as follows:
2. the compound alkalescent phenol resin solidifying agent of one according to claim 1, is characterized in that: the preparation method of described many methylolureas mixture is as follows:
Urea and formaldehyde are reacted to 2～2.5h at 85～90 DEG C, obtain described many methylolureas mixture.
3. the compound alkalescent phenol resin solidifying agent of one according to claim 2, is characterized in that: the mol ratio of described urea and formaldehyde is 1.2～1.5:1.
4. the compound alkalescent phenol resin solidifying agent of one according to claim 1, is characterized in that: described carbonate is one or both in sodium carbonate and salt of wormwood.
5. the compound alkalescent phenol resin solidifying agent of one according to claim 1, is characterized in that: described organic esters is more than one in ethyl acetate, propylene carbonate, glycerol acetate and methyl-formiate.
6. a preparation method for compound alkalescent phenol resin solidifying agent as claimed in claim 1, is characterized in that: described method steps is as follows:
Successively many methylolureas mixture, water and carbonate are put in reactor, stirred, add polyvinyl alcohol and organic esters, stir, obtain described composite phenol formaldehyde tree solidifying agent.
7. a compound alkalescent phenol resin solidifying agent as claimed in claim 1 is applied to solidifying of resol.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106398106A (en) * | 2016-05-16 | 2017-02-15 | 北京林业大学 | Phenolic resin composite curing agent for artificial board, and application thereof |
| CN106883800A (en) * | 2017-03-31 | 2017-06-23 | 中国林业科学研究院木材工业研究所 | A kind of Resin adhesive and preparation method thereof |
| CN109517330A (en) * | 2018-11-22 | 2019-03-26 | 山东莱芜润达新材料有限公司 | A kind of preparation method of phenol formaldehyde foam resin curing agent |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343382A (en) * | 2008-08-22 | 2009-01-14 | 辽宁福鞍铸业集团有限公司 | Organic ester solidifying agent for alkalescent phenolic resin |
-
2014
- 2014-09-02 CN CN201410442679.XA patent/CN104212123B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343382A (en) * | 2008-08-22 | 2009-01-14 | 辽宁福鞍铸业集团有限公司 | Organic ester solidifying agent for alkalescent phenolic resin |
Non-Patent Citations (1)
| Title |
|---|
| 陈玉竹等: "酚醛树脂复合型固化剂的可行性初探", 《南京林业大学学报（自然科学版）》, vol. 38, no. 4, 28 August 2014 (2014-08-28) * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106398106A (en) * | 2016-05-16 | 2017-02-15 | 北京林业大学 | Phenolic resin composite curing agent for artificial board, and application thereof |
| CN106398106B (en) * | 2016-05-16 | 2018-11-06 | 北京林业大学 | A kind of compound curing agent of wood-based plate phenolic resin and its application |
| CN106883800A (en) * | 2017-03-31 | 2017-06-23 | 中国林业科学研究院木材工业研究所 | A kind of Resin adhesive and preparation method thereof |
| CN109517330A (en) * | 2018-11-22 | 2019-03-26 | 山东莱芜润达新材料有限公司 | A kind of preparation method of phenol formaldehyde foam resin curing agent |
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