CN102604019A - Preparation method and device and application of resorcinol-formaldehyde resins - Google Patents
Preparation method and device and application of resorcinol-formaldehyde resins Download PDFInfo
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- CN102604019A CN102604019A CN2012100605490A CN201210060549A CN102604019A CN 102604019 A CN102604019 A CN 102604019A CN 2012100605490 A CN2012100605490 A CN 2012100605490A CN 201210060549 A CN201210060549 A CN 201210060549A CN 102604019 A CN102604019 A CN 102604019A
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Abstract
The invention relates to a preparation method and device and application of resorcinol-formaldehyde resin. The preparation method comprises the following specific steps: (1) adding resorcinol, formaldehyde and a solvent into an upper reactor of a reaction device in sequence and stirring and heating the materials; (2) slowly adding catalysts when the temperature in the upper reactor reaches 28-30 DEG C; and mixing the catalysts with the reaction solution uniformly; (3) then carrying out catalytic reaction, thus obtaining a preliminary reaction solution; (4) leaching the preliminary reaction solution to obtain a secondary reaction solution; and (5) ensuring the secondary reaction solution to enter a lower reactor via a valve plate at the bottom of the upper reactor and stirring and distilling the secondary reaction solution through heating, thus obtaining the alkylphenol-formaldehyde resin. The resin is a reinforcing agent of natural rubbers and synthetic rubbers, is soluble in alcohols, lipids and the like and is convenient to use.
Description
[technical field]
The present invention relates to the fine chemical technology field, specifically, is a kind of preparation method and device and application of resorcinol formaldehyde resin.
[background technology]
Phenol formaldehyde resin, with a kind of resol that phenol and formaldehyde condensation polymer make, its product performance and main application: this resin is mainly used in the chloroprene rubber adhesive agent industry.Also as the butyl rubber vulcanizing agent, and frie retardant coating, printing ink, adhesive tape, molding powder, stratified plastics; Make varnish or insulation, corrosion resistant coating; Make daily necessities, ornamental; Make sound insulation, lagging material etc.Common high voltage electric socket, the production of furniture plastic handles.Accumulating condition: put shady and cool dry place, avoid the moisture absorption, prevent periods of direct sunlight, keep fire away.
[summary of the invention]
The objective of the invention is to overcome the deficiency of prior art, a kind of preparation method and device and application of resorcinol formaldehyde resin are provided.
The objective of the invention is to realize through following technical scheme:
A kind of preparation method of resorcinol formaldehyde resin, its concrete steps are:
(1) with Resorcinol, formaldehyde, solvent join in the upper strata reactor drum of reaction unit successively, carry out stirring heating;
(2) when the temperature in the reactor drum of upper strata arrives 28～30 ℃, slowly add catalyzer; Catalyzer and reaction solution are mixed;
(3) carry out catalyzed reaction then, then obtain initial reaction liquid;
The condition of catalyzed reaction is: the reaction times is 8～12h, and temperature of reaction is 55～65 ℃,
(4) initial reaction liquid is carried out suction filtration; Obtain secondary reaction liquid;
(5) lower valve plates of secondary reaction liquid through the upper strata reactor drum entered into lower reactor, stir and add thermal distillation, promptly obtain resorcinol formaldehyde resin.
Described Heating temperature is 115～125 ℃;
The mass percent of described formaldehyde is 35%;
Described solvent is methyl alcohol or methanol in water;
The mol ratio of described Resorcinol and formaldehyde is 1: 1.4～1.8; Be preferably 1: 1.6;
Described catalyzer is an anionite-exchange resin, is preferably strongly basic anion exchange resin, and ion-exchange equivalent is greater than 5;
Described catalyst consumption is 82～88% of a Resorcinol quality, is preferably 85%;
This color of resin is the reddish-brown granular solids, and its softening temperature is 80～110 ℃;
In addition, the present invention can also provide a kind of preparation method of phenol formaldehyde resin,
Described Resorcinol replaces with phenol, and the product of final preparation is a phenol formaldehyde resin; This color of resin is yellow to the transparent granular solids of brown, and its softening temperature is 80～110 ℃.
A kind of preparation facilities of resorcinol formaldehyde resin, described reaction unit is made up of upper strata reactor drum and lower reactor, and lower reactor is positioned at the bottom of upper strata reactor drum; Link to each other through pipeline between the last valve plate of upper strata reactor drum and the lower valve plate of lower reactor, be provided with middle valve plate in the middle of the pipeline, the upper and lower ends of middle valve plate is respectively equipped with filter screen;
Described filter screen is more than 2;
Flowing of the reaction solution of described valve plate control levels reactor drum;
Described filter screen can be changed or clean as required; Help the removal of reaction impurities; This is one of bright spot of the present invention.
Compared with prior art, positively effect of the present invention is:
(1) this resin is tree elastomer and elastomeric strengthening agent, can be used for tire, fields such as travelling belt.
(2) this resin dissolves in alcohols, and lipid etc. are easy to use;
(3) this resins process is integrated carries out, and economizes on resources, and avoids contaminate environment;
(4) this resin is widely used, and can use fields such as various chemical materials.
[description of drawings]
All schematic representation of apparatus of Fig. 1 the present invention;
Label in the accompanying drawing is respectively: 1 opening for feed, and 2 upper strata reactor drums, 3 distillers, 4 stirring rod, 5 supports, 6 stirring rakes, 7 lower reactor, 8 thermopairs, 9 discharge ports, 10 times air outlets, 11 lower valve plates, valve plate in 12,13 filter screens, valve plate on 14, on 15 the air outlet.
[embodiment]
The preparation method of a kind of resorcinol formaldehyde resin of the present invention and the embodiment of application below are provided.
The reaction unit that present embodiment is used: be made up of upper strata reactor drum 2 and lower reactor 7, lower reactor is positioned at the bottom of upper strata reactor drum; Link to each other through pipeline between the last valve plate 14 of upper strata reactor drum and the lower valve plate 11 of lower reactor, valve plate 12 in being provided with in the middle of the pipeline, the upper and lower ends of middle valve plate is respectively equipped with filter screen 13;
Described filter screen is more than two;
Described upper strata reactor drum also is respectively equipped with opening for feed 1 and last air outlet 15;
Described upper strata reactor drum and lower reactor also are provided with a thermopair 8, are used for reacting by heating liquid;
Described upper strata reactor drum and lower reactor also are provided with a whisking appliance, and wherein the support 5 of whisking appliance is fixed on the top board of upper strata reactor drum and lower reactor, and stirring rod 4 lower ends connect stirring rake 6;
Described lower reactor also is respectively equipped with discharge port 9 and following air outlet 10;
Described lower reactor also is respectively equipped with distiller 3; Be chemical industry distiller 3 commonly used;
Flowing of the reaction solution of described valve plate control levels reactor drum;
Described filter screen can be changed or clean as required; Help the removal of reaction impurities;
A kind of preparation method of resorcinol formaldehyde resin, its concrete steps are:
(1) with Resorcinol, formaldehyde, solvent join in the upper strata reactor drum of reaction unit successively, carry out stirring heating;
(2) when the temperature in the reactor drum of upper strata arrives 28 ℃, slowly add catalyzer; Catalyzer and reaction solution are mixed;
(3) carry out catalyzed reaction then, then obtain initial reaction liquid;
The condition of catalyzed reaction is: the reaction times is 8h, and temperature of reaction is 55 ℃,
(4) initial reaction liquid is carried out suction filtration; Obtain secondary reaction liquid;
(5) lower valve plates of secondary reaction liquid through the upper strata reactor drum entered into lower reactor, stir and add thermal distillation, promptly obtain resorcinol formaldehyde resin.
Described Heating temperature is 115 ℃;
The mass percent of described formaldehyde is 35%;
Described solvent is methyl alcohol or methanol in water;
The mol ratio of described Resorcinol and formaldehyde is 1: 1.4;
Described catalyzer is an anionite-exchange resin, is preferably strongly basic anion exchange resin, and ion-exchange equivalent is greater than 5;
Described catalyst consumption is 82% of a Resorcinol quality;
This color of resin is the reddish-brown granular solids, and its softening temperature is 80 ℃.
A kind of preparation method of resorcinol formaldehyde resin, its concrete steps are:
(1) with Resorcinol, formaldehyde, solvent join in the upper strata reactor drum of reaction unit successively, carry out stirring heating;
(2) when the temperature in the reactor drum of upper strata arrives 29 ℃, slowly add catalyzer; Catalyzer and reaction solution are mixed;
(3) carry out catalyzed reaction then, then obtain initial reaction liquid;
The condition of catalyzed reaction is: the reaction times is 10h, and temperature of reaction is 60 ℃,
(4) initial reaction liquid is carried out suction filtration; Obtain secondary reaction liquid;
(5) lower valve plates of secondary reaction liquid through the upper strata reactor drum entered into lower reactor, stir and add thermal distillation, promptly obtain resorcinol formaldehyde resin.
Described Heating temperature is 120 ℃;
The mass percent of described formaldehyde is 35%;
Described solvent is methyl alcohol or methanol in water;
The mol ratio of described Resorcinol and formaldehyde is 1: 1.6;
Described catalyzer is an anionite-exchange resin, is preferably strongly basic anion exchange resin, and ion-exchange equivalent is greater than 5;
Described catalyst consumption is 85% of a Resorcinol quality;
This color of resin is the reddish-brown granular solids, and its softening temperature is 95 ℃.
A kind of preparation method of resorcinol formaldehyde resin, its concrete steps are:
(1) with Resorcinol, formaldehyde, solvent join in the upper strata reactor drum of reaction unit successively, carry out stirring heating;
(2) when the temperature in the reactor drum of upper strata arrives 30 ℃, slowly add catalyzer; Catalyzer and reaction solution are mixed;
(3) carry out catalyzed reaction then, then obtain initial reaction liquid;
The condition of catalyzed reaction is: the reaction times is 12h, and temperature of reaction is 65 ℃,
(4) initial reaction liquid is carried out suction filtration; Obtain secondary reaction liquid;
(5) lower valve plates of secondary reaction liquid through the upper strata reactor drum entered into lower reactor, stir and add thermal distillation, promptly obtain resorcinol formaldehyde resin.
Described Heating temperature is 125 ℃;
The mass percent of described formaldehyde is 35%;
Described solvent is methyl alcohol or methanol in water;
The mol ratio of described Resorcinol and formaldehyde is 1.8
Described catalyzer is an anionite-exchange resin, is preferably strongly basic anion exchange resin, and ion-exchange equivalent is greater than 5;
Described catalyst consumption is 88% of a Resorcinol quality;
This color of resin is the reddish-brown granular solids, and its softening temperature is 110 ℃.
Embodiment 4
A kind of preparation method of phenol formaldehyde resin, its concrete steps are:
(1) with phenol, formaldehyde, solvent join in the upper strata reactor drum of reaction unit successively, carry out stirring heating;
(2) when the temperature in the reactor drum of upper strata arrives 30 ℃, slowly add catalyzer; Catalyzer and reaction solution are mixed;
(3) carry out catalyzed reaction then, then obtain initial reaction liquid;
The condition of catalyzed reaction is: the reaction times is 12h, and temperature of reaction is 65 ℃,
(4) initial reaction liquid is carried out suction filtration; Obtain secondary reaction liquid;
(5) lower valve plates of secondary reaction liquid through the upper strata reactor drum entered into lower reactor, stir and add thermal distillation, promptly obtain the alkylphenol formaldehyde resin resinoid.
Described Heating temperature is 125 ℃;
The mass percent of described formaldehyde is 35%;
Described solvent is methyl alcohol or methanol in water;
The mol ratio of described phenol and formaldehyde is 1.8
Described catalyzer is an anionite-exchange resin, is preferably strongly basic anion exchange resin, and ion-exchange equivalent is greater than 5;
Described catalyst consumption is 88% of a phenol quality;
This color of resin is yellow to the transparent granular solids of brown, and its softening temperature is 90 ℃.
A kind of preparation method of phenol formaldehyde resin, its concrete steps are:
(1) with phenol, formaldehyde, solvent join in the upper strata reactor drum of reaction unit successively, carry out stirring heating;
(2) when the temperature in the reactor drum of upper strata arrives 29 ℃, slowly add catalyzer; Catalyzer and reaction solution are mixed;
(3) carry out catalyzed reaction then, then obtain initial reaction liquid;
The condition of catalyzed reaction is: the reaction times is 10h, and temperature of reaction is 60 ℃,
(4) initial reaction liquid is carried out suction filtration; Obtain secondary reaction liquid;
(5) lower valve plates of secondary reaction liquid through the upper strata reactor drum entered into lower reactor, stir and add thermal distillation, promptly obtain phenol formaldehyde resin.
Described Heating temperature is 120 ℃;
The mass percent of described formaldehyde is 35%;
Described solvent is methyl alcohol or methanol in water;
The mol ratio of described phenol and formaldehyde is 1: 1.6;
Described catalyzer is an anionite-exchange resin, is preferably strongly basic anion exchange resin, and ion-exchange equivalent is greater than 5;
Described catalyst consumption is 85% of a phenol quality;
This color of resin is yellow to the transparent granular solids of brown, and its softening temperature is 100 ℃.
The above only is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the present invention's design; Can also make some improvement and retouching, these improvement and retouching also should be regarded as in protection scope of the present invention.
Claims (10)
1. the preparation method of a resorcinol formaldehyde resin is characterized in that, its concrete steps are:
(1) with Resorcinol, formaldehyde, solvent join in the upper strata reactor drum of reaction unit successively, carry out stirring heating;
(2) when the temperature in the reactor drum of upper strata arrives 28～30 ℃, slowly add catalyzer; Catalyzer and reaction solution are mixed;
(3) carry out catalyzed reaction then, then obtain initial reaction liquid;
The condition of catalyzed reaction is: the reaction times is 8～12h, and temperature of reaction is 55～65 ℃,
(4) initial reaction liquid is taken out suction filtration; Obtain secondary reaction liquid;
(5) lower valve plates of secondary reaction liquid through the upper strata reactor drum entered into lower reactor, stir and add thermal distillation, promptly obtain alkylphenol formaldehyde resin;
Described Heating temperature is 115～125 ℃;
The mass percent of described formaldehyde is 35%;
Described solvent is methyl alcohol or methanol in water;
The mol ratio of described Resorcinol and formaldehyde is 1: 1.4～1.8;
Described catalyzer is an anionite-exchange resin, and ion-exchange equivalent is greater than 5;
Described catalyst consumption is 82～88% of a Resorcinol quality.
2. the preparation method of a kind of resorcinol formaldehyde resin as claimed in claim 1 is characterized in that, the mol ratio of described Resorcinol and formaldehyde 1: 1.6.
3. the preparation method of a kind of resorcinol formaldehyde resin as claimed in claim 1 is characterized in that, described catalyzer is for being strongly basic anion exchange resin.
4. the preparation method of a kind of resorcinol formaldehyde resin as claimed in claim 1 is characterized in that, described catalyst consumption is 85% of a Resorcinol quality.
5. the preparation facilities of a resorcinol formaldehyde resin is characterized in that, described reaction unit is made up of upper strata reactor drum and lower reactor, and lower reactor is positioned at the bottom of upper strata reactor drum; Link to each other through pipeline between the last valve plate of upper strata reactor drum and the lower valve plate of lower reactor, be provided with middle valve plate in the middle of the pipeline, the upper and lower ends of middle valve plate is respectively equipped with filter screen; The number of filter screen is more than two.
6. the preparation facilities of a kind of resorcinol formaldehyde resin as claimed in claim 5 is characterized in that,
Described upper strata reactor drum and lower reactor also are provided with a thermopair;
Described upper strata reactor drum and lower reactor also are provided with a whisking appliance, and wherein the support of whisking appliance is fixed on the top board of upper strata reactor drum and lower reactor, and the stirring rod lower end connects stirring rake.
7. the preparation facilities of a kind of resorcinol formaldehyde resin as claimed in claim 5 is characterized in that,
Described upper strata reactor drum also be respectively equipped with opening for feed and on give vent to anger.
8. the preparation facilities of a kind of resorcinol formaldehyde resin as claimed in claim 5 is characterized in that,
Described lower reactor also is respectively equipped with discharge port and following air outlet;
Described lower reactor also is respectively equipped with distiller.
9. the preparation method of a kind of resorcinol formaldehyde resin as claimed in claim 1 is characterized in that, described Resorcinol or phenol, and the product of final preparation is a phenol formaldehyde resin.
10. the application of resorcinol formaldehyde resin in field of rubber materials.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100605490A CN102604019A (en) | 2012-03-08 | 2012-03-08 | Preparation method and device and application of resorcinol-formaldehyde resins |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100605490A CN102604019A (en) | 2012-03-08 | 2012-03-08 | Preparation method and device and application of resorcinol-formaldehyde resins |
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| CN102604019A true CN102604019A (en) | 2012-07-25 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2012100605490A Pending CN102604019A (en) | 2012-03-08 | 2012-03-08 | Preparation method and device and application of resorcinol-formaldehyde resins |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103087284A (en) * | 2012-11-14 | 2013-05-08 | 江苏国立化工科技有限公司 | Preparation method of alkylresorcinol formaldehyde resin |
| CN107459614A (en) * | 2017-08-28 | 2017-12-12 | 上海超程化工科技有限公司 | A kind of environment-friendly type adhesion promotor and preparation method thereof, application |
-
2012
- 2012-03-08 CN CN2012100605490A patent/CN102604019A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103087284A (en) * | 2012-11-14 | 2013-05-08 | 江苏国立化工科技有限公司 | Preparation method of alkylresorcinol formaldehyde resin |
| CN107459614A (en) * | 2017-08-28 | 2017-12-12 | 上海超程化工科技有限公司 | A kind of environment-friendly type adhesion promotor and preparation method thereof, application |
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Application publication date: 20120725 |