CN104311764A - Novel water soluble phenolic resin adhesive synthetic process - Google Patents
Novel water soluble phenolic resin adhesive synthetic process Download PDFInfo
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- CN104311764A CN104311764A CN201410491697.7A CN201410491697A CN104311764A CN 104311764 A CN104311764 A CN 104311764A CN 201410491697 A CN201410491697 A CN 201410491697A CN 104311764 A CN104311764 A CN 104311764A
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Abstract
The invention discloses a novel water soluble phenolic resin adhesive synthetic process, and relates to the technical field of chemical industry; a water soluble phenolic resin adhesive is obtained through carrying out a full reaction of a colorless phenol crystal molten by heating with a sodium hydroxide aqueous solution (0.1 mol/L) and formaldehyde. The synthetic process has the beneficial effects that the synthetic process has the advantages of convenient and simple preparation, environmental protection, no pollution, easy availability of raw materials, less equipment investment, pure quality, and convenient operation; and the prepared water soluble phenolic resin adhesive is good in use effect, safe and reliable.
Description
Technical field
The present invention relates to chemical technology field, be specifically related to a kind of novel water-soluble phenolic resin adhesive synthesis technique.
Background technology
Resol is industrialized synthetic resins the earliest, is also the synthetic adhesive first occurred, or the first sqtructural adhesive that modification is obtained, at first for aircraft industry.Although the appearance of novel adhesive, in a lot of, instead of synvaren, because of the particular advantages of itself, its importance did not still subtract originally, still had larger development and application.Resol polarity is comparatively large, and to metal with majority is nonmetal good cementability, bonding strength is higher.Owing to there is a large amount of phenyl ring in resol, can be cross-linked into body structure again, rigidity is comparatively large, and thus thermotolerance is high, creep resistance, resistance to ablation, good stability of the dimension.Water-fast, oil resistant, wear-resisting, resistant to chemical media, resistance to mould, ageing-resistant etc., electrical insulation capability is excellent, apply very extensive, but in the technique of current industrial production Phenol aldehyde resin, all there is the problems such as yield is low, purity not high pollution is serious, and production technique is comparatively complicated, be difficult to meet human wants.
Summary of the invention
It is high that technical problem to be solved by this invention is to provide a kind of quality, the water-soluble phenolic resin adhesive synthesis technique that preparation technology is simply novel.
Technical problem to be solved by this invention realizes by the following technical solutions:
Novel water-soluble phenolic resin adhesive synthesis technique, is characterized in that: comprise following processing step,
A. the three-necked flask of a 500ml is chosen as reaction flask.
B. take the colourless phenol crystal of 45-50g and be heated to 40-45 DEG C, being added after its fusing in the reaction flask in step a, starting to stir.
C. the aqueous sodium hydroxide solution (0.1mol/L) taking 120-130ml adds in the reaction flask in above-mentioned steps b, temperature to be controlled at 40-50 DEG C of isothermal reaction 20-30min after particle appears in inside when its solution pinkiness.
D. the formaldehyde taking 48-49g is thrown in the reaction flask in above-mentioned steps c, after stirring 2-4min, temperature is continued remain on 45-50 DEG C of isothermal reaction 25-35min, in 80min, then has 50 DEG C to rise to 87 DEG C, then after 25min rises to 95 DEG C by 87 DEG C insulation reaction 20min.
E. by 95 DEG C, 82 DEG C are cooled to above-mentioned reacted solution in 30min, again add the formaldehyde insulation reaction 10-20min of 12-12.5g.
F., after above-mentioned steps e reaction terminates, in 30min, temperature is risen to 92 DEG C of insulation reaction 5-10min by 82 DEG C again.
G. treat that in above-mentioned steps f, in reaction flask, solution is rendered as glue, when color is dark-brown, solution temperature is controlled at 92-96 DEG C of insulation 15-25min.
H., after above-mentioned steps g reaction terminates, it is (100-200) * 10 that sample thief detects viscosity
-5m
2s
-1time, pass into water coolant and cool, when temperature is down to 40 DEG C, start discharging, the dark brown viscous liquid obtained is water-soluble phenolic resin adhesive finished product.
The invention has the beneficial effects as follows: the present invention is simply easy to prepare, environment friendly and pollution-free, raw material is easy to get, and facility investment is few, and quality is pure, convenient operation, and the water-soluble phenolic resin adhesive result of use of preparation is good, safe and reliable.
Embodiment
The technique means realized to make the present invention, creation characteristic, reaching object and effect is easy to understand, below in conjunction with specific embodiment, setting forth the present invention further.
Embodiment 1
Novel water-soluble phenolic resin adhesive synthesis technique, comprises following processing step,
A. the three-necked flask of a 500ml is chosen as reaction flask.
B. take the colourless phenol crystal of 45g and be heated to 40 DEG C, being added after its fusing in the reaction flask in step a, starting to stir.
C. the aqueous sodium hydroxide solution (0.1mol/L) taking 120ml adds in the reaction flask in above-mentioned steps b, temperature to be controlled at 40 DEG C of isothermal reaction 20-30min after particle appears in inside when its solution pinkiness.
D. the formaldehyde taking 48g is thrown in reaction flask in above-mentioned steps c, after stirring 2min, temperature is continued to remain on 45 DEG C of isothermal reaction 25min, in 80min, then has 50 DEG C to rise to 87 DEG C, then after 25min rises to 95 DEG C by 87 DEG C insulation reaction 20min.
E. by 95 DEG C, 82 DEG C are cooled to above-mentioned reacted solution in 30min, again add the formaldehyde insulation reaction 10min of 12-12.5g.
F., after above-mentioned steps e reaction terminates, in 30min, temperature is risen to 92 DEG C of insulation reaction 5min by 82 DEG C again.
G. treat that in above-mentioned steps f, in reaction flask, solution is rendered as glue, when color is dark-brown, solution temperature is controlled at 92 DEG C of insulation 15min.
H., after above-mentioned steps g reaction terminates, it is (100-200) * 10 that sample thief detects viscosity
-5m
2s
-1time, pass into water coolant and cool, when temperature is down to 40 DEG C, start discharging, the dark brown viscous liquid obtained is water-soluble phenolic resin adhesive finished product.
Embodiment 2
Novel water-soluble phenolic resin adhesive synthesis technique, comprises following processing step,
A. the three-necked flask of a 500ml is chosen as reaction flask.
B. take the colourless phenol crystal of 47g and be heated to 43 DEG C, being added after its fusing in the reaction flask in step a, starting to stir.
C. the aqueous sodium hydroxide solution (0.1mol/L) taking 125ml adds in the reaction flask in above-mentioned steps b, temperature to be controlled at 45 DEG C of isothermal reaction 20-30min after particle appears in inside when its solution pinkiness.
D. the formaldehyde taking 48.4g is thrown in reaction flask in above-mentioned steps c, after stirring 3min, temperature is continued to remain on 48 DEG C of isothermal reaction 30min, in 80min, then has 50 DEG C to rise to 87 DEG C, then after 25min rises to 95 DEG C by 87 DEG C insulation reaction 20min.
E. by 95 DEG C, 82 DEG C are cooled to above-mentioned reacted solution in 30min, again add the formaldehyde insulation reaction 15min of 12.1g.
F., after above-mentioned steps e reaction terminates, in 30min, temperature is risen to 92 DEG C of insulation reaction 5-10min by 82 DEG C again.
G. treat that in above-mentioned steps f, in reaction flask, solution is rendered as glue, when color is dark-brown, solution temperature is controlled at 94 DEG C of insulation 20min.
H., after above-mentioned steps g reaction terminates, it is (100-200) * 10 that sample thief detects viscosity
-5m
2s
-1time, pass into water coolant and cool, when temperature is down to 40 DEG C, start discharging, the dark brown viscous liquid obtained is water-soluble phenolic resin adhesive finished product.
More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (1)
1. novel water-soluble phenolic resin adhesive synthesis technique, is characterized in that: comprise following processing step,
A. the three-necked flask of a 500ml is chosen as reaction flask.
B. take the colourless phenol crystal of 45-50g and be heated to 40-45 DEG C, being added after its fusing in the reaction flask in step a, starting to stir.
C. the aqueous sodium hydroxide solution (0.1mol/L) taking 120-130ml adds in the reaction flask in above-mentioned steps b, temperature to be controlled at 40-50 DEG C of isothermal reaction 20-30min after particle appears in inside when its solution pinkiness.
D. the formaldehyde taking 48-49g is thrown in the reaction flask in above-mentioned steps c, after stirring 2-4min, temperature is continued remain on 45-50 DEG C of isothermal reaction 25-35min, in 80min, then has 50 DEG C to rise to 87 DEG C, then after 25min rises to 95 DEG C by 87 DEG C insulation reaction 20min.
E. by 95 DEG C, 82 DEG C are cooled to above-mentioned reacted solution in 30min, again add the formaldehyde insulation reaction 10-20min of 12-12.5g.
F., after above-mentioned steps e reaction terminates, in 30min, temperature is risen to 92 DEG C of insulation reaction 5-10min by 82 DEG C again.
G. treat that in above-mentioned steps f, in reaction flask, solution is rendered as glue, when color is dark-brown, solution temperature is controlled at 92-96 DEG C of insulation 15-25min.
H., after above-mentioned steps g reaction terminates, it is (100-200) * 10 that sample thief detects viscosity
-5m
2s
-1time, pass into water coolant and cool, when temperature is down to 40 DEG C, start discharging, the dark brown viscous liquid obtained is water-soluble phenolic resin adhesive finished product.
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CN201410491697.7A CN104311764A (en) | 2014-09-23 | 2014-09-23 | Novel water soluble phenolic resin adhesive synthetic process |
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CN201410491697.7A CN104311764A (en) | 2014-09-23 | 2014-09-23 | Novel water soluble phenolic resin adhesive synthetic process |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105601859A (en) * | 2016-01-19 | 2016-05-25 | 宜兴市宇球保温材料有限公司 | Water-soluble phenol-formaldehyde resin glue for rock wool and preparation method thereof |
CN106380560A (en) * | 2016-08-31 | 2017-02-08 | 李芹 | Formula and preparation technology of water-soluble phenolic resin glue |
CN111844275A (en) * | 2020-07-15 | 2020-10-30 | 浙江雁杰建筑模板有限公司 | Manufacturing method of outer wall panel of bamboo green integrated house |
CN115044001A (en) * | 2022-06-20 | 2022-09-13 | 安徽进化硅纳米材料科技有限公司 | Method for producing water-soluble phenolic resin and co-producing aqueous calcium carbonate suspension by using white carbon black wastewater |
-
2014
- 2014-09-23 CN CN201410491697.7A patent/CN104311764A/en active Pending
Non-Patent Citations (1)
Title |
---|
罗娟等: "水溶性酚醛树脂胶的制备", 《化学与粘合》 * |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105601859A (en) * | 2016-01-19 | 2016-05-25 | 宜兴市宇球保温材料有限公司 | Water-soluble phenol-formaldehyde resin glue for rock wool and preparation method thereof |
CN106380560A (en) * | 2016-08-31 | 2017-02-08 | 李芹 | Formula and preparation technology of water-soluble phenolic resin glue |
CN111844275A (en) * | 2020-07-15 | 2020-10-30 | 浙江雁杰建筑模板有限公司 | Manufacturing method of outer wall panel of bamboo green integrated house |
CN111844275B (en) * | 2020-07-15 | 2022-03-25 | 浙江雁杰建筑模板有限公司 | Manufacturing method of outer wall panel of bamboo green integrated house |
CN115044001A (en) * | 2022-06-20 | 2022-09-13 | 安徽进化硅纳米材料科技有限公司 | Method for producing water-soluble phenolic resin and co-producing aqueous calcium carbonate suspension by using white carbon black wastewater |
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Application publication date: 20150128 |