CN1064083A - Process for preparing reinforced resin - Google Patents
Process for preparing reinforced resin Download PDFInfo
- Publication number
- CN1064083A CN1064083A CN 92106073 CN92106073A CN1064083A CN 1064083 A CN1064083 A CN 1064083A CN 92106073 CN92106073 CN 92106073 CN 92106073 A CN92106073 A CN 92106073A CN 1064083 A CN1064083 A CN 1064083A
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- qualified
- phenol
- reinforced resin
- acidic catalyst
- preparing reinforced
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Abstract
The present invention relates to a kind of process for preparing reinforced resin that is used for rubber and goods thereof.It adopts raw material phenol, formaldehyde under an acidic catalyst effect, insulation heats up in polymeric kettle, refluxes, after treating that the control softening temperature is qualified, residual water is drawn in the static separation of water-cooled stopped reaction, material is heated up pour in the still kettle again, after treating that free phenol is qualified, be put into normal pressure intensification in the finished product still, decompression dehydration gets final product the film releasing discharging after four hours then.It is not only easy and simple to handle, and technical process is short, and is energy-conservation, non-environmental-pollution, and obviously improve the quality of products and yield, significantly reduce raw materials cost and production cost.
Description
The present invention relates to a kind of process for preparing reinforced resin that is used for rubber and goods thereof.
Reinforced resin is used widely as the strengthening agent of rubber and goods thereof.It can not only improve the hardness of rubber item and the sticking power of rubber and metal, produces top-quality rubber steel wire meridian tire and automobile anti-skid chain, also can be used for aspects such as electrical material, emery wheel manufacturing, printing, paper product processing.But the production technique of existing reinforced resin is to adopt solvent-extraction process, produces needs though its product can satisfy, and also has problem anxious to be solved.One raw material mixed solvent consumption is big, and especially the consumption of butanols is bigger, and the smell of solvent impairs HUMAN HEALTH to the pollution of environment in operating process; Its two mixed solvent recycles in extracting resin process, wherein all is being mingled with the free phenol of different content at every turn, easily causes pollution once more to product with the resin of this solvent extraction, thereby influences the qualification rate of free phenol item technical indicator in the product; Recycling of its three mixed solvent can cause solvent burden ratio out of proportion, influences the result of use of solvent, in use occurs the emulsion of resin sometimes, makes troubles to production operation; Its four extractions resin is repeatedly washed, and causes with resin liquid and runs off, and reduces the yield of product, increases energy consumption, prolongs technical process, has improved manufacturing cost.
The purpose of this invention is to provide a kind of process for preparing reinforced resin of producing, it is not only easy and simple to handle, and technical process is short, and is energy-conservation, non-environmental-pollution, and obviously improve the quality of products and yield, significantly reduce raw materials cost and production cost.
The object of the present invention is achieved like this: produce 100 parts of the raw materials used weight ratio phenol of reinforced resin, formaldehyde 64-92 part, an acidic catalyst 0.1-10 part, earlier the phenol after formaldehyde and the dissolving is dropped in the polymeric kettle and heat up, adding an acidic catalyst intensification simultaneously stirs, when temperature rises to 90-100 ℃, insulation 1-2 hour refluxes, after middle control softening temperature is qualified, residual water is drawn in the static separation of water-cooled stopped reaction, material is warming up to 70-80 ℃ again and pours into and carry out vapor distillation in the still kettle, after treating that free phenol content is qualified, be put into normal pressure intensification dehydration in the finished product still, when temperature rises to 125-135 ℃, be decompressed to 0.08-0.1Mpa, temperature remains on 135-140 ℃, can the film releasing discharging after four hours.
Because the present invention adopts under an acidic catalyst effect, directly carry out the vapor distillation dehydration behind Pyrogentisinic Acid, the formaldehyde reaction and extract resin, so not only easy and simple to handle, technical process is short, and, material-saving more energy-conservation than conventional solvent extraction method, non-environmental-pollution.This technology has fundamentally solved the problem that solvent-extraction process exists.At first novel process has been cancelled the mixed solvent that distributes contaminate environment in the manufacturing processed, is detrimental to health, effectively avoided the resin emulsion that occurs in recycling that the solvent burden ratio that causes is out of proportion and causing using because of mixed solvent, thereby save a large amount of solvents, obviously improve the quality of products, significantly reduce cost.Directly dewater in addition with vapor distillation, the technology that recycles, repeatedly washes, dewaters without mixed solvent, significantly reduce the free phenol that is mingled with in the loss of resin and the resin, obviously improved the qualification rate of free phenol item technical indicator in product yield and the product, gone back water-saving, power saving, saving of labor.Therefore, process for preparing reinforced resin of the present invention is better than existing solvent extraction process especially, is easy to apply.Wherein an acidic catalyst can adopt oxalic acid, hydrochloric acid, phosphoric acid etc. as catalyzer according to actual needs.
The invention will be further described below in conjunction with embodiment.
Example 1: take by weighing raw material according to quantity,, mix to drop in the polymeric kettle and heat up earlier with 400 parts of phenol, dissolving back and 322 parts in formaldehyde, drop into 3.6 parts of oxalic acid (concentration 10%) simultaneously, be warming up to 95 ℃ of insulations 1.5 hours that reflux, after middle control softening temperature is qualified, residual water is drawn in the static separation of water-cooled stopped reaction.Again material is warming up to 75 ℃ and pours into and carry out vapor distillation in the still kettle, treat that free phenol content is qualified after, be put in the finished product still normal pressure dehydration that heats up, when temperature rises to 130-135 ℃, carry out decompression dehydration, be decompressed to 0.08-0.1Mpa, temperature remains on 135-140 ℃.Can the film releasing discharging after four hours.
Detected result:
95 ℃ of softening temperatures
Free phenol 0.6%
360 parts of output
Yield 90%(is in phenol)
Example 2: take by weighing raw material according to quantity, earlier with 400 parts of phenol, dissolving back and 314 parts in formaldehyde, mix to drop in the polymeric kettle and heat up, drop into 2.2 parts of oxalic acid (concentration 10%) simultaneously, be warming up to 90 ℃ of insulations 1 hour that reflux, drop into 1.4 parts of oxalic acid (concentration 10%) again, be incubated 20 minutes, after middle control softening temperature was qualified, residual water was drawn in the static separation of water-cooled stopped reaction.Again material is warming up to 75 ℃ and pours into and carry out vapor distillation in the still kettle, treat that free phenol content is qualified after, be put in the finished product still normal pressure dehydration that heats up, when temperature rises to 125-130 ℃, carry out decompression dehydration, be decompressed to 0.08-0.1Mpa, temperature remains on 135-140 ℃.Can the film releasing discharging after four hours.
Detected result:
100 ℃ of softening temperatures
Free phenol 0.85%
370 parts of output
Yield 93%(is in phenol)
Claims (2)
1, a kind of process for preparing reinforced resin, it is characterized in that: 100 parts of raw materials used weight ratio phenol, formaldehyde 64-92 part, an acidic catalyst 0.1-10 part, earlier the phenol after formaldehyde and the dissolving is dropped in the polymeric kettle and heat up, adding an acidic catalyst intensification simultaneously stirs, when temperature rises to 90-100 ℃, refluxing is incubated 1-2 hour, after middle control softening temperature is qualified, and the static separation of water-cooled stopped reaction, draw residual water, again material is warming up to 70-80 ℃ and pours into and carry out vapor distillation in the still kettle, treat that free phenol content is qualified after, be put in the finished product still normal pressure dehydration that heats up, when temperature rises to 125-135 ℃, be decompressed to 0.08-0.1Mpa, temperature remains on 135-140 ℃, can the film releasing discharging after four hours.
2, process for preparing reinforced resin according to claim 1 is characterized in that: described an acidic catalyst is selected oxalic acid, hydrochloric acid or phosphoric acid for use.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92106073 CN1064083A (en) | 1992-03-03 | 1992-03-03 | Process for preparing reinforced resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92106073 CN1064083A (en) | 1992-03-03 | 1992-03-03 | Process for preparing reinforced resin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1064083A true CN1064083A (en) | 1992-09-02 |
Family
ID=4941767
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92106073 Pending CN1064083A (en) | 1992-03-03 | 1992-03-03 | Process for preparing reinforced resin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1064083A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101113194B (en) * | 2007-08-09 | 2010-07-07 | 山东圣泉化工股份有限公司 | Highly-water-soluble thermosetting phenolic resin and method for synthesizing the same |
-
1992
- 1992-03-03 CN CN 92106073 patent/CN1064083A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101113194B (en) * | 2007-08-09 | 2010-07-07 | 山东圣泉化工股份有限公司 | Highly-water-soluble thermosetting phenolic resin and method for synthesizing the same |
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| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |