CN1271164C - Dipping glue for papreg and preparing method thereof - Google Patents
Dipping glue for papreg and preparing method thereof Download PDFInfo
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- CN1271164C CN1271164C CN 200510070308 CN200510070308A CN1271164C CN 1271164 C CN1271164 C CN 1271164C CN 200510070308 CN200510070308 CN 200510070308 CN 200510070308 A CN200510070308 A CN 200510070308A CN 1271164 C CN1271164 C CN 1271164C
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- glue
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- 239000003292 glue Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000007598 dipping method Methods 0.000 title abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical group O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 36
- 238000001816 cooling Methods 0.000 claims description 10
- 150000001299 aldehydes Chemical class 0.000 claims description 9
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 5
- 230000000739 chaotic effect Effects 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 4
- 239000005416 organic matter Substances 0.000 claims description 4
- 238000003860 storage Methods 0.000 claims description 4
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 150000001896 cresols Chemical class 0.000 claims description 2
- 125000002256 xylenyl group Chemical class C1(C(C=CC=C1)C)(C)* 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims 3
- 229930013930 alkaloid Natural products 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 6
- 229920000877 Melamine resin Polymers 0.000 abstract description 5
- 238000005034 decoration Methods 0.000 abstract description 4
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 abstract description 3
- 238000007711 solidification Methods 0.000 abstract description 2
- 230000008023 solidification Effects 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract 2
- 230000008030 elimination Effects 0.000 abstract 1
- 238000003379 elimination reaction Methods 0.000 abstract 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 abstract 1
- 238000004879 turbidimetry Methods 0.000 abstract 1
- 235000019256 formaldehyde Nutrition 0.000 description 11
- 229920005989 resin Polymers 0.000 description 11
- 239000011347 resin Substances 0.000 description 11
- 239000010410 layer Substances 0.000 description 10
- 239000003063 flame retardant Substances 0.000 description 5
- 239000002344 surface layer Substances 0.000 description 5
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 239000004640 Melamine resin Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 150000001912 cyanamides Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- -1 is that Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 229920003987 resole Polymers 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Paper (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The present invention relates to paper layer press plate dipping glue and a production method thereof. The paper layer press plate dipping glue is composed of the following raw materials (by weight portion): 250 to 500 portions of phenol organics., 5o to 500 portions of melamine., 500 to 1000 portions of aldehyde organics., 100 to 800 portions of solvents and 3 to 20 portions of catalysts; the raw materials are weighed firstly according to the requirement for the weight portion ratio, and are added and stirred in a reaction vessel, and a pH value is adjusted by the addition of the catalysts; after the temperature is uniformly raised to 40 to 45 DEG C, the melamine is added, and the temperature continues to rise. At the temperature of 90 to 95 DEG C, the temperature is kept for 30 minutes, and then, the water-soluble factor determination or water turbidimetry is carried out; in the simultaneous process, the reaction temperature is kept for 40 to 60 minutes; the temperature immediately drops, and an amount of solvent is added; after the temperature drops to 45 DEC C, discharged materials are final products. The dipping glue is especially suitable for being used as the dipping glue of a paper layer press plate for decoration, and has the advantages of enhanced fire retardance and comprehensive quality of laminated poles, low cost, no generation of free phenol at the time of solidification, elimination of trouble of environmental protection, etc.
Description
Technical field
The present invention relates to the binder composition and the production method thereof of thin laminates such as Mierocrystalline cellulose, plastic construction.
Background technology
The thin layer product of Mierocrystalline cellulose or plastic construction such as surface-mounted integrated circuit, consolidated floor, papery decorative sheet etc., surface-mounted integrated circuit is that application of epoxy or unsaturated polyester resin and cloth dipping are pressed in the traditional method; The consolidated floor skin-material is to form with resin impregnating hot pressing; The papery decorative sheet adds functional agent dipping lamination again with resol, top layer and forms.In the prior art, the employing of above-mentioned conventional adhesive, the burst size height of formaldehyde is difficult to satisfy environmental requirement, and production cost is higher, does not reach the index of high flame retardant level PLASTIC LAMINATED.
CN97114693.4 discloses U.S. Premark PWP Holdings, Inc. " method of coating melamine resin on laminated paper " patent in China's application, capable the illustrating of its specification sheets page 1 6-16 is to be applied on the decoration paper of doing the top layer with " melamine resin ", again with the central layer lamination of using resin impregnating, to improve wear resistance, flame retardant resistance and tinctorial property.The dipping glue of its core still is phenol formaldehyde resin glue.And this patent does not provide the production method of any relevant melamine glue.
By retrieval, do not find interference applications of the present invention, do not find the commercially available product of this dipping glue yet in China market.
Summary of the invention
The present invention is directed to the above-mentioned deficiency of prior art, design a kind of burst size of methanal is lower, compliance with environmental protection requirements, reduce production costs, improve flame retardant properties paper-based laminate dipping glue and production method thereof.
Above-mentioned purpose can realize with following measure: it is made up of following raw material and weight part thereof: 250-500 part phenol organic matter, 50-500 part trimeric cyanamide, 500-1000 part aldehydes organism, 100-800 part solvent, 3-20 part catalyzer; Earlier with the phenolic material of fusing and aldehydes by weight proportion requirement weigh, (formaldehyde can once always add or divide 2-3 adding to add the reactor stirring, need therebetween to heat up respectively, insulation, cooling), adding catalyzer transfers pH value to 8.0-9.5, evenly heat up, the still temperature rise adds trimeric cyanamide during to 40-45 ℃ and heats up, the control heat-up rate, after in the time of 90-95 ℃, being incubated 30 minutes, carry out molten water multiple mensuration or water chaotic degree and measure, the molten water multiple when 20 ℃ of water temperatures is to 1-0.7 times, or water chaotic degree is checked when globe is arranged, terminal point is promptly arrived in reaction, the insulation of process reaction therebetween 40-60 minute, cooling adds an amount of solvent immediately, when being cooled to 45 ℃, blowing is finished product.
The also available following measure of above-mentioned purpose comes perfect: said phenol organic matter is at least a in cresols, xylenol, the nonyl phenol etc.; Said aldehydes organism is formaldehyde and/or furfural; Said solvent is at least a in methyl alcohol, ethanol, the water; Said catalyzer is NaoH, KOH, Ba (OH)
2, at least a in the bases thing such as ammoniacal liquor.
Embodiment
The present invention will now be further detailed embodiment: raw material and the weight part proportioning thereof with ten embodiment is listed as into following table earlier.
Embodiment 1 (consulting weight part proportioning numeral in the table):
Earlier (as select nonyl phenol for use phenol, fusing earlier) furfural of 400 weight parts and 600 weight parts adds the reactor stirring, add that about 8 weight part NaoH transfer pH value evenly to be warming up to 40-45 ℃ to 8.0-9.5, adding 300 weight part trimeric cyanamides again continues to heat up, but need the control heat-up rate, be incubated during to 90-95 ℃, and note measuring and the control pH value, be incubated after 30 minutes, carrying out the mensuration or the water chaotic degree of molten water multiple measures, when water temperature during at 20 ℃ molten water multiple to 1-0.7 doubly or the opacity check when globe is arranged reaction arrived terminal point, the insulation of process reaction therebetween 45-60 minute, cooling adds 650 parts by weight of ethanol immediately, and blowing finishes when cooling to 45 ℃.
Embodiment 2-10 can make this dipping glue with embodiment 1 identical method by the weight part proportioning of last each raw material of table.
To be considered as a whole according to the physicochemical property of the degree of perfection of the height of cost, reaction, the dipping glue that makes and the key elements such as advantages and disadvantages that these performances bring for production, environmental protection, benefit as for the selected of the size of the proportional quantity of each material composition.Added as phenolic material, though plasticity-enhanced advantage is arranged, the trouble of the environmental protection that has free phenol to increase to bring; Fire-retardant, attrition resistant advantage that trimeric cyanamide has, but hardness and fragility are big, the poor stability of glue; Aldehydes has been added the degree of crosslinking height, has been become glue fast, but release formaldehyde is unfavorable to HUMAN HEALTH; Solvent is many cost-saving but tackiness is poor; Catalyzer is too much very few all can to cause waste.Selecting a kind of or several problems in aldehydes matter, the aldehyde material, mainly is that, colloid amount simplified and traditional from cost, technology considered and decided.Amid all these factors, the present invention is preferred with embodiment 1,6,7,9.
Scheme with embodiment 9 is that example is described further below, and the dipping glue outward appearance of making is a beige homogeneous transparent colloidal liquid, and storage period, pH value was 8-9 greater than three months, and free phenol is 8-10%, and free formaldehyde is less than 0.8%.
This dipping glue application method on the decoration paper-based laminate is: adopt the direct method gum dipping process, make the paper substrate two sides be subjected to glue, by liquid squeezing roll and paper substrate travelling speed control impregnation resin content, drying baker adopts steam heating, hot air circulation makes gummed paper evenly dry, gets rid of solvent.Paper substrate travelling speed per minute 10-15 rice, 90～100 ℃ of oven temperatures, final gel content 30g/m
2
Whole heat pressing process is: intensification preheating-insulation-intensification-constant temperature-cooling, and unit pressure 5-7Mpa, concrete grammar is as follows:
Pre-heating stage: temperature begins temperature from room temperature to the surface layer curing reaction, and the sandwich layer resin is heated simultaneously, and the discharge section volatile matter, and exerting pressure is 1/3～1/2 of total head.Rate of heating 2-4 ℃/minute, to 80 ℃.
Holding stage: make the surface layer tree refer under than low reaction speed, solidify.The fusing of sandwich layer resin thermally equivalent, beginning is merged mutually between the resin layer interface.Be incubated 5-10 minute down at 100 ℃.
Temperature rise period: continue to keep 2-4 ℃ of/minute heat-up rate, enter constant temperature to 140-150 ℃.By solidifying the top temperature of stipulating when the beginning temperature rises to compacting, heat-up rate is unsuitable too fast, otherwise can make the surface layer curing speed too fast, can not cause finished product layering or crackle with the fine fusion of sandwich layer resin.
The constant temperature stage: after temperature reaches maximum, keep the constant stage, the effect in this stage is to guarantee that the surface layer resin fully solidifies, the sandwich layer resin evenly plastifies, and guarantee adhere between each layered material sheet, making it under pressure is an even closely knit integral body, and then makes end properties reach optimum value.Between 140-150 ℃, kept 10-15 minute, cool off after the end.
Cooling stages: the surface layer resin fully solidifies in slab, and after fully merging with the sandwich layer resin, the cooling of can lowering the temperature, the refrigerative method is a logical water coolant in the hot plate of press, also can naturally cooling.This stage should carry out under the pressure that keeps regulation, and controls suitable speed of cooling.Can the release demoulding when plate temperature drops to below 60 ℃.
Free phenol to this decoration paper matter veneer sheet dipping glue is measured the GB/T14074.13-93 standard that adopts, and free formaldehyde mensuration adopts the GB/T14074.16-93 standard; The sheet material burst size of methanal is measured and is adopted moisture eliminator method among the GB/T 17657-99, combustionproperty to adopt GB/T 2406-93 standard.
The outward appearance of sheet material meets GB/T 7911-99 standard, density 1.30g/cm
3, water-intake rate 3.51%, Rockwell hardness: M110, tensile strength is greater than 80MPa, flexural strength 79MPa, notched Izod impact strength 2.6KJ/m
2, oxygen index: 48.0, anti-boiling water boils 2hr: no layering, bubbling, weightening finish thickens less than 3% less than 5%.Sheet material burst size of methanal (moisture eliminator method) is less than 1.5mg/L.
Can find out that from the reaction process of this dipping glue after trimeric cyanamide had hydroxyl, phenol and formaldehyde had increased Pyrogentisinic Acid's building-up reactions chance in polycondensation process, thereby had reduced the generation of free phenol to a certain extent.We account for phenol, formaldehyde to the add-on of trimeric cyanamide and add 40% o'clock of total amount, carry out anti-storage, sheet material incendivity, tensile strength, anti-boiling water and boil performance and test and compare, and consequently: storage period was greater than three months; Oxygen index reaches 48; Tensile strength and tradition dipping matrix this maintain an equal level (greater than 80MPa); It is not stratified that anti-boiling water boils performance, no bubbling, and weightening finish thickens less than 3% less than 5%.
The present invention compares existing phenolic impregnated glue, and flame retardant properties and integrated quality improve, and substitutes more phenol with trimeric cyanamide, and the ton valency of glue is reduced to 5800 yuan by 6500 yuan, and price advantage is obvious, and does not produce free phenol in the solidification process, eliminates a kind of trouble of environmental protection.
This glue also can be used in the production of surface-mounted integrated circuit, consolidated floor, medium density fibre board (MDF), automobile brake sheet.
When specific embodiments of the present invention disclosed one by one, obviously, various other improvement were accomplished to one skilled in the art easily, and this also is difficult to depart from the spirit and scope of the invention, were futile just as the alternative of equivalent of generally acknowledging.Embodiment does not comprise the whole of claims limited field yet, and this also is that patent work person knows together.
Claims (6)
1, a kind of paper-based laminate immersion glue production method is characterized in that this glue is made up of following raw material and weight part thereof: 250-500 part phenol organic matter, 50-500 part trimeric cyanamide, 500-1000 part aldehydes organism, 100-800 part solvent, 3-20 part catalyzer; Earlier with the phenolic material of fusing and aldehydes by weight proportion requirement weigh, adding reactor stirs, adding catalyzer transfers pH value to 8.0-9.5, evenly heat up, the still temperature rise adds trimeric cyanamide during to 40-45 ℃ and heats up, the control heat-up rate, in the time of 90-95 ℃, be incubated 30 minutes after, carry out that molten water multiple is measured or water chaotic degree is measured, molten water multiple when 20 ℃ of water temperatures to 1-0.7 doubly, or water chaotic degree check is when having globe, and terminal point promptly arrive in reaction, and the insulation of process reaction therebetween is 40-60 minute, cooling immediately, the solvent that adds the 100-800 weight part, when being cooled to 45 ℃, blowing is finished product.
2, paper-based laminate immersion glue production method as claimed in claim 1 is characterized in that said phenol organic matter is at least a in cresols, xylenol, the nonyl phenol.
3, paper-based laminate immersion glue production method as claimed in claim 1 is characterized in that said aldehydes organism is formaldehyde and/or furfural.
4, paper-based laminate immersion glue production method as claimed in claim 1 is characterized in that said solvent is at least a in methyl alcohol, ethanol, the water.
5, paper-based laminate immersion glue production method as claimed in claim 1 is characterized in that said catalyzer is to be selected from least a in sodium hydroxide, potassium hydroxide, ammoniacal liquor, four kinds of alkaloids of hydrated barta.
6, the glue that makes of paper-based laminate immersion glue production method as claimed in claim 1 is characterized in that this glue outward appearance is a beige homogeneous transparent colloidal liquid, and storage period, PH=8-9, free phenol were 8-10%, free formaldehyde＜0.8% greater than three months.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510070308 CN1271164C (en) | 2005-04-28 | 2005-04-28 | Dipping glue for papreg and preparing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510070308 CN1271164C (en) | 2005-04-28 | 2005-04-28 | Dipping glue for papreg and preparing method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1687285A CN1687285A (en) | 2005-10-26 |
| CN1271164C true CN1271164C (en) | 2006-08-23 |
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ID=35305327
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200510070308 Expired - Fee Related CN1271164C (en) | 2005-04-28 | 2005-04-28 | Dipping glue for papreg and preparing method thereof |
Country Status (1)
| Country | Link |
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| CN (1) | CN1271164C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100402572C (en) * | 2006-01-24 | 2008-07-16 | 浙江林学院 | Production method of melamine and bamboo wood phenol liquified substance modified phenolic resin |
| CN100554580C (en) * | 2007-08-21 | 2009-10-28 | 浙江玲珑装饰材料有限公司 | Paper flame-proof decorative plate and immersion glue production method thereof |
| CN104140777A (en) * | 2013-05-07 | 2014-11-12 | 合肥安诺新型建材有限公司 | Formaldehyde-free impregnated paper laminated decorating plate and preparation method thereof |
| CN114960294A (en) * | 2022-06-01 | 2022-08-30 | 上海贝辉木业有限公司 | Anti-cracking impregnated paper and preparation method thereof |
-
2005
- 2005-04-28 CN CN 200510070308 patent/CN1271164C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1687285A (en) | 2005-10-26 |
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