CN117547854A - Resin synthesis process solid powder raw material recrystallization method and application - Google Patents
Resin synthesis process solid powder raw material recrystallization method and application Download PDFInfo
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- CN117547854A CN117547854A CN202311519883.2A CN202311519883A CN117547854A CN 117547854 A CN117547854 A CN 117547854A CN 202311519883 A CN202311519883 A CN 202311519883A CN 117547854 A CN117547854 A CN 117547854A
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- 239000000843 powder Substances 0.000 title claims abstract description 75
- 239000002994 raw material Substances 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 58
- 239000007787 solid Substances 0.000 title claims abstract description 40
- 239000011347 resin Substances 0.000 title claims abstract description 30
- 229920005989 resin Polymers 0.000 title claims abstract description 30
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 28
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 28
- 238000001953 recrystallisation Methods 0.000 title claims abstract description 16
- 230000008018 melting Effects 0.000 claims abstract description 28
- 238000002844 melting Methods 0.000 claims abstract description 28
- 239000013078 crystal Substances 0.000 claims abstract description 26
- 239000002245 particle Substances 0.000 claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
- 238000000859 sublimation Methods 0.000 claims abstract description 8
- 230000008022 sublimation Effects 0.000 claims abstract description 8
- 238000002425 crystallisation Methods 0.000 claims abstract description 5
- 230000008025 crystallization Effects 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 238000009834 vaporization Methods 0.000 claims abstract description 3
- 230000008016 vaporization Effects 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 26
- 230000003247 decreasing effect Effects 0.000 claims description 4
- 238000007790 scraping Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 238000004140 cleaning Methods 0.000 abstract description 6
- 239000002904 solvent Substances 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 description 4
- 239000003814 drug Substances 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
Abstract
The invention discloses a recrystallization method and application of a resin synthesis process solid powder raw material, wherein the method comprises the following steps: s1, treating a solid powder raw material of a resin synthesis process in a low-temperature crystallization mode, wherein the sublimation temperature is the melting point temperature of the powder raw material, and recrystallizing the powder raw material in a low-temperature region after high-temperature vaporization in a sublimator; s2, grinding and crushing the recrystallized bulk crystals to form crystal particles with uniform shapes and particle sizes. According to the recrystallization method and application of the resin synthesis process solid powder raw material, the solid fine powder is changed into crystal particles with uniform particle size from powder, so that the problems that the solid powder is stuck on the inner wall of a pipeline in the production process, so that the pipeline is blocked, the metering accuracy of automatic metering equipment is affected, and the product quality is affected due to the fact that the solid powder is stuck on the inner wall of a reaction kettle are solved; meanwhile, the problems that the solvent is wasted in the cleaning process of the reaction kettle and resin raw materials exist in corners to cause the cleaning in place are solved, and the production cost is reduced.
Description
Technical Field
The invention relates to the technical field of solid powder raw material treatment, in particular to a resin synthesis process solid powder raw material recrystallization method and application.
Background
In recent years, with the continuous development of science and technology, mechanical equipment requiring feeding has begun to implement an automated operation mode. That is, a mature feeder needs to be used to complete the feeding process. Vacuum powder feeders are now widely used in production processes, working in either high or low temperature environments. Therefore, the technical advantages are quite outstanding in the process of product feeding. As far as its function is concerned, it will continue to move towards the specialization trend. The vacuum powder feeding process is mature, and the vacuum powder feeding machine has strong conveying capacity and high conveying efficiency in terms of the effect, so that the working efficiency of most industrial production processes is greatly improved.
According to the existing production condition, in the process of vacuum feeding and automatic metering feeding of solid powder, the solid powder is extremely easy to adhere to a transmission pipeline and an automatic metering system due to static electricity of the powder and contact of the inner wall of the pipeline, metering errors and pipeline blockage are caused, and dust can be generated when the solid powder enters a reaction kettle and adheres to the inner wall of the reaction kettle. In the past, the damage of an automatic metering system is extremely easy to cause, and serious errors are caused to the production and feeding amount, so that the quality of products is seriously influenced, and even the condition of unqualified products is caused.
Disclosure of Invention
The invention aims to provide a recrystallization method and application of a resin synthesis process solid powder raw material, which solve the problem that dust is generated when solid powder enters a reaction kettle and adheres to the inner wall of the reaction kettle.
In order to achieve the above object, the present invention provides a method for recrystallizing a solid powder raw material in a resin synthesis process, comprising the steps of:
s1, treating a solid powder raw material of a resin synthesis process in a low-temperature crystallization mode, wherein the sublimation temperature is the melting point temperature of the powder raw material, and recrystallizing the powder raw material in a low-temperature region after high-temperature vaporization in a sublimator;
s2, grinding and crushing the recrystallized bulk crystals to form crystal particles with uniform shapes and particle sizes.
Preferably, a resin synthesis process solid powder raw material recrystallization method comprises the following steps:
s2-1, placing a solid powder raw material of a resin synthesis process into a zone B of an eight-temperature zone sublimator, setting the temperature of the zone B as the melting point temperature of the powder raw material, increasing the temperature of the zone A by 0-10 ℃ for the melting point temperature of the powder raw material, and sequentially decreasing the melting point temperature of the powder raw material by 0-40 ℃ for zones C, D, E, F, G and H to enable the sublimated raw material to be secondarily crystallized in the zone D-H;
s2-2, scraping off the bulk crystal raw materials in the D region-H region after sublimation is completed, and respectively storing; before feeding, the bulk crystal raw material is ground to have the particle size of 5 mu m, and the ground crystal particles are packaged and transported to an automatic feeding system for production.
Therefore, the recrystallization method and application of the resin synthesis process solid powder raw material have the following technical effects:
(1) The material is changed into small crystal particles from solid powder, so that the problems of blocking a pipeline, sticking on the inner wall of a reaction kettle and affecting the metering accuracy of an automatic metering system in the production-process of the powder are reduced;
(2) The material is sublimated, so that the content of metal ions contained in the material can be reduced, and the purity of the material is improved; through testing, the purity of the material can be improved to 99.9 percent, and the method can be widely applied to the semiconductor industry and the medicine industry with higher requirements on raw materials and products;
(3) The material adhesion and electrostatic force are reduced, the improvement and the improvement of the automatic process of the production line are facilitated, the manpower resource cost is reduced, the full-automatic production operation is realized, and the production efficiency is improved;
(4) The problem that the pipeline is blocked by materials is solved, the pipeline cleaning and purging frequency is reduced, unnecessary raw material waste is reduced, and the labor and material cost in the cleaning process is reduced;
(5) Solves the problem of material sticking on the inner wall of the reaction kettle, is favorable for ensuring the accuracy and stability of production and feeding and ensures the stable quality of products; meanwhile, the problems of solvent waste and incomplete cleaning caused by resin raw materials and the like in corners in the cleaning process of the reaction kettle are reduced, and the production cost is reduced.
The technical scheme of the invention is further described in detail through examples.
Detailed Description
The technical scheme of the invention is further described below by examples.
Unless defined otherwise, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs.
Example 1
A recrystallization method of solid powder raw material in resin synthesis process is characterized in that the solid powder raw material in resin synthesis process is DA0035, DA0035 is gray powder, and the melting temperature is 305 ℃.
50G of DA0035 was placed in a Dan Yingliao boat of an eight temperature zone sublimator, dan Yingliao boat being zone B, zone B being set to 305℃of the melting point of the powder feedstock, zone A being set to 315℃of the melting point of the powder feedstock, zone C being set to 300℃of the melting point, zone D being set to 260℃of the melting point of the powder feedstock, zone E being set to 240℃of the melting point of the powder feedstock, zone F being set to 200℃of the melting point of the powder feedstock, zone G being set to 160℃of the melting point of the powder feedstock, and zone H being set to 120 ℃.
The temperature of the zone A is higher than the melting point temperature, so that the crystallization of the raw materials in the zone A in front of a material boat is prevented, the movement of the raw materials from a high temperature zone to a low temperature zone after the raw materials are melted is ensured, the temperature of the zone C-H is sequentially reduced, and the secondary crystallization of the materials in the zone D-H is ensured.
After the sublimation was completed for 24 hours, the bulk crystal raw material in the D region to H region was scraped off, and the crystal raw material was ground to a size of 5 μm using a grinder to obtain crystal particles a.
Example two
A recrystallization method of resin synthesis process solid powder raw material is provided, wherein the resin synthesis process solid powder raw material is DM0230, DM0230 is soil gray solid, and the melting temperature is 270 ℃.
4500G of DM0230 was placed in a Dan Yingliao boat of an eight temperature zone sublimator, dan Yingliao boat was zone B, zone B was set to 270℃of melting point of powder raw material, zone A was set to 280℃of temperature, zone C was set to 238℃of temperature, zone D was set to 220℃of temperature, zone E was set to 210℃of temperature, zone F was set to 170℃of temperature, zone G was set to 130℃of temperature, and zone H was set to 90 ℃.
After the completion of sublimation for 48 hours, the bulk crystal raw material in the D region to H region was scraped off, and the crystal raw material was ground to a size of 5 μm using a grinder to obtain crystal particles B.
Example III
A recrystallization method of solid powder raw material in resin synthesis process comprises DA0079, DA0079 is yellow powder, and melting temperature is 380 ℃.
10G of DA0079 was placed in a Dan Yingliao boat of an eight-temperature zone sublimator, dan Yingliao boat being zone B, zone B being 380℃at the melting point of the powder raw material, zone A being 390℃at the temperature of zone C being 360℃at the temperature of zone D being 320℃at the temperature of zone E being 320℃at the temperature of zone F being 280℃at the temperature of zone G being 240℃and zone H being 200 ℃.
After the sublimation was completed for 24 hours, the bulk crystal raw material in the D region to H region was scraped off, and the crystal raw material was ground to a size of 5 μm using a grinder to obtain crystal particles C.
Test
(1) The states, yields and purities of the crystal grains obtained in examples one to three are shown in table 1.
TABLE 1 State, yield and purity of Crystal particles
The preparation method can improve the purity of the materials to 99.9 percent, and can be widely applied to the semiconductor industry and the medicine industry with higher requirements on raw materials and products
(2) The ion content changes before and after recrystallization of the solid powder raw material in the resin synthesis process in examples one to three are shown in table 2, and the ion content analysis equipment is ICP-MS:
TABLE 2 ion Change before and after recrystallization of powder raw materials
The method shows that the contents of metal ions and nonmetal ions in the raw materials treated by the preparation method are reduced, and the method has great influence on improving the purity of the materials, ensuring the stability of the quality of the products and improving the application range of the products.
Therefore, the invention adopts the recrystallization method and the application of the resin synthesis process solid powder raw material, changes the solid fine powder into crystal particles with uniform particle size from powder, and solves the problems that the solid powder is stuck on the inner wall of a pipeline in the production process, so that the pipeline is blocked, the metering accuracy of automatic metering equipment is affected, and the product quality is affected by sticking on the inner wall of a reaction kettle.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting it, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that: the technical scheme of the invention can be modified or replaced by the same, and the modified technical scheme cannot deviate from the spirit and scope of the technical scheme of the invention.
Claims (5)
1. The recrystallization method of the solid powder raw material in the resin synthesis process is characterized by comprising the following steps of:
s1, treating a solid powder raw material of a resin synthesis process in a low-temperature crystallization mode, wherein the sublimation temperature is the melting point temperature of the powder raw material, and recrystallizing the powder raw material in a low-temperature region after high-temperature vaporization in a sublimator;
s2, grinding and crushing the recrystallized bulk crystals to form crystal particles with uniform shapes and particle sizes.
2. A method for recrystallizing a solid powder material for a resin synthesis process according to claim 1, comprising the steps of:
s2-1, placing a solid powder raw material of a resin synthesis process into a zone B of an eight-temperature zone sublimator, setting the temperature of the zone B as the melting point temperature of the powder raw material, increasing the temperature of the zone A by 0-10 ℃ for the melting point temperature of the powder raw material, and sequentially decreasing the melting point temperature of the powder raw material by 0-40 ℃ for zones C, D, E, F, G and H to enable the sublimated raw material to be secondarily crystallized in the zone D-H;
s2-2, scraping off the bulk crystal raw materials in the D region-H region after sublimation is completed, and respectively storing; before feeding, the bulk crystal raw material is ground to have the particle size of 5 mu m, and the ground crystal particles are packaged and transported to an automatic feeding system for production.
3. The method for recrystallizing solid powder material in resin synthesis process according to claim 1, wherein in step S2-1, the solid powder material in resin synthesis process is placed in zone B of the eight-temperature zone sublimator, zone B is set to be the melting point temperature of the powder material, zone a is 10 ℃ higher than the melting point temperature of the powder material, zone C, zone D, zone E, zone F, zone G and zone H are successively decreased by 0 to 40 ℃ from the melting point temperature of the powder material, and the sublimated material is secondarily crystallized in zone D to zone H.
4. The method for recrystallizing solid powder material in resin synthesis process according to claim 1, wherein in step S2-1, the solid powder material in resin synthesis process is placed in zone B of the eight-temperature zone sublimator, zone B is set to be the melting point temperature of the powder material, zone a is 10 ℃ higher than the melting point temperature of the powder material, zone C, zone D, zone E, zone F, zone G and zone H are successively decreased by 20-40 ℃ from the melting point temperature of the powder material, and the sublimated material is secondarily crystallized in zone D-zone H.
5. Use of a recrystallization method according to any one of claims 1 to 4 for the treatment of solid powder raw materials in a resin synthesis process.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311519883.2A CN117547854A (en) | 2023-11-15 | 2023-11-15 | Resin synthesis process solid powder raw material recrystallization method and application |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311519883.2A CN117547854A (en) | 2023-11-15 | 2023-11-15 | Resin synthesis process solid powder raw material recrystallization method and application |
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| CN117547854A true CN117547854A (en) | 2024-02-13 |
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| CN202311519883.2A Pending CN117547854A (en) | 2023-11-15 | 2023-11-15 | Resin synthesis process solid powder raw material recrystallization method and application |
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| Country | Link |
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- 2023-11-15 CN CN202311519883.2A patent/CN117547854A/en active Pending
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