CN117776872A - Preparation method for co-production of 98% pentaerythritol and 99% pentaerythritol - Google Patents
Preparation method for co-production of 98% pentaerythritol and 99% pentaerythritol Download PDFInfo
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- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 title claims abstract description 233
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 229940059574 pentaerithrityl Drugs 0.000 claims description 229
- 239000013078 crystal Substances 0.000 claims description 72
- 239000000706 filtrate Substances 0.000 claims description 69
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 68
- 239000000463 material Substances 0.000 claims description 65
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims description 48
- 238000006460 hydrolysis reaction Methods 0.000 claims description 38
- 230000007062 hydrolysis Effects 0.000 claims description 37
- 238000003756 stirring Methods 0.000 claims description 35
- 238000001914 filtration Methods 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 28
- 238000002156 mixing Methods 0.000 claims description 26
- 229940098779 methanesulfonic acid Drugs 0.000 claims description 24
- 229910052799 carbon Inorganic materials 0.000 claims description 23
- 239000000843 powder Substances 0.000 claims description 22
- 239000012043 crude product Substances 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 17
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 12
- 244000060011 Cocos nucifera Species 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000002023 wood Substances 0.000 claims description 11
- TXBCBTDQIULDIA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)CO TXBCBTDQIULDIA-UHFFFAOYSA-N 0.000 claims description 8
- 238000002425 crystallisation Methods 0.000 claims description 8
- 230000008025 crystallization Effects 0.000 claims description 8
- PTJWCLYPVFJWMP-UHFFFAOYSA-N 2-[[3-hydroxy-2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)COCC(CO)(CO)CO PTJWCLYPVFJWMP-UHFFFAOYSA-N 0.000 claims description 7
- 238000004042 decolorization Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 5
- 239000000243 solution Substances 0.000 description 53
- 239000000203 mixture Substances 0.000 description 35
- 239000000047 product Substances 0.000 description 29
- 239000012535 impurity Substances 0.000 description 25
- 238000006243 chemical reaction Methods 0.000 description 22
- 238000001816 cooling Methods 0.000 description 20
- 238000004090 dissolution Methods 0.000 description 20
- 239000012452 mother liquor Substances 0.000 description 20
- 238000003825 pressing Methods 0.000 description 17
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 7
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 230000003301 hydrolyzing effect Effects 0.000 description 6
- 239000002075 main ingredient Substances 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000006482 condensation reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000010413 mother solution Substances 0.000 description 2
- AJUSPBSXOGUAFJ-UHFFFAOYSA-N 2-(hydroxymethyl)-2-(methoxymethyl)propane-1,3-diol Chemical compound COCC(CO)(CO)CO AJUSPBSXOGUAFJ-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 241000219495 Betulaceae Species 0.000 description 1
- 238000005705 Cannizzaro reaction Methods 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000004280 Sodium formate Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 125000002777 acetyl group Chemical class [H]C([H])([H])C(*)=O 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 description 1
- 235000019254 sodium formate Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a preparation method for co-producing 99% of pentaerythritol by 98% of pentaerythritol, which relates to the technical field of basic chemical industry.
Description
Technical Field
The invention relates to the technical field of basic chemical industry, in particular to a preparation method for co-producing 99% pentaerythritol by 98% of pentaerythritol.
Background
Pentaerythritol (PE) is a white powdery crystal, is easily esterified by common organic acid, is widely used for producing alkyd resin, synthetic high-grade lubricant, plasticizer, surfactant, medicine and explosive in the paint industry, and is an important chemical raw material. At present, the industrial production of pentaerythritol mainly adopts a sodium method, namely, the pentaerythritol is prepared by condensation reaction of formaldehyde and acetaldehyde in the presence of a sodium hydroxide alkaline catalyst, and sodium formate is produced as a byproduct. The method for synthesizing the pentaerythritol is carried out in two steps, wherein the first Alder reaction is an endothermic reaction, the second Cannizzaro reaction is an exothermic reaction, the temperature rise reaction is required to be gentle in the condensation process, otherwise, side reactions can occur, byproducts are increased, the product yield is reduced, the difficulty of the subsequent separation process is increased, and the yield and quality of the pentaerythritol are affected.
For the past years, many methods for preparing pentaerythritol by using formaldehyde and acetaldehyde as raw materials, such as CN105111047A, CN109438182A and the like report that condensation reaction is performed under the catalysis of liquid alkali. However, by-products such as pentaerythritol formal, methyl alcohol-pentaerythritol acetal, pentaerythritol methyl ether and the like are generated in the condensation reaction process, and the pentaerythritol content is low, so that the product quality is affected. CN103044199a reports that phosphoric acid is used as a catalyst, 95% grade pentaerythritol is hydrolyzed into 98% grade pentaerythritol at high temperature and high pressure, but pentaerythritol needs to be treated in advance before hydrolysis, so the process is designed to be continuous in and out, a hydrolysis tower is used as a core reactor, a large amount of water washing is needed, and the investment of production cost is increased.
Aiming at the problems existing in the prior art, it is necessary to find a preparation method for co-producing 98% pentaerythritol and 99% pentaerythritol, which has the advantages of good product quality, low cost and less loss.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides a preparation method for co-producing 98% pentaerythritol and 99% pentaerythritol, which can achieve the aim of simultaneously producing 98% pentaerythritol and 99% pentaerythritol under the conditions of impure raw materials and low acidity.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the invention provides a preparation method for co-producing 99% pentaerythritol by 98% pentaerythritol, which comprises the following steps:
(1) Mixing water and the pentaerythritol crude, regulating the pH value to obtain a pentaerythritol solution I, and then heating and pressurizing for hydrolysis to obtain a hydrolysis material I;
(2) Decolorizing, press-filtering, crystallizing and press-filtering the hydrolysis material I obtained in the step (1) again to obtain a crystal I and a filtrate I, and drying the crystal I to obtain 98% pentaerythritol;
(3) Mixing the crystal I obtained in the step (2) with a pentaerythritol crude product, regulating the pH value to obtain a pentaerythritol solution II, and heating and pressurizing to hydrolyze to obtain a hydrolysis material II;
(4) Decolorizing, press-filtering, crystallizing and press-filtering the hydrolysis material II obtained in the step (3) again to obtain a crystal II and a filtrate II;
(5) And (3) drying the crystal II obtained in the step (4) to obtain 99% pentaerythritol.
Further, the 98% pentaerythritol is specifically about 98% by mass of pentaerythritol, and the 99% pentaerythritol is specifically about 99% by mass of pentaerythritol.
Further, the crude pentaerythritol product in the step (1) comprises 85-90% of monopentaerythritol, 3-5% of dipentaerythritol, 0.5-1% of tripentaerythritol and the balance of water.
Further, the pH of the first pentaerythritol solution in the step (1) is 2-2.5; the pH of the pentaerythritol solution II in the step (3) is 2.5-3.
Further, in the step (1), the weight ratio of the water to the pentaerythritol crude is 3-5:1; preferably 3:1.
Further, the temperature of the heating in the steps (1) and (3) is 110-140 ℃ and the time is 3-6h; the pressure of the pressurized hydrolysis is 0.1-0.3Mpa; the conditions for decoloring in the steps (2) and (4) are as follows: the temperature is 90-110 ℃ and the time is 15min, and the pressure is normal; the crystallization temperatures in the steps (2) and (4) are 30-50 ℃ and the crystallization time is 3-6h.
Further, the decolorization in the steps (2) and (4) is carried out by adding active carbon specifically, and the particle size is 100-200 meshes; the addition amount of the activated carbon in the step (2) is 1.0-2.0% of the total weight of the pentaerythritol crude, and the addition amount of the activated carbon in the step (2) is 2.0-4.0% of the total weight of the pentaerythritol crude.
Further, the activated carbon comprises coconut shell powder activated carbon and/or wood powder activated carbon.
Further, when the stirring rate of the crystallization in the step (4) is 5-10r/min, the crystal size is 40-80 meshes; when the stirring speed is 10-20r/min, the crystal size is 80-100 meshes; when the stirring speed is above 20r/min, the crystal size is 100-200 meshes.
Further, the filtrate I in the step (2) and the filtrate II in the step (4) are returned to the preparation process of the pentaerythritol solution I in the step (1) and/or the preparation process of the pentaerythritol solution II in the step (3) to replace water for use.
Further, the weight ratio of the second filtrate, the first crystals and the crude pentaerythritol in the step (3) is 5-7:1:1, preferably 6:1:1.
In some specific embodiments, the preparation method for co-producing 99% pentaerythritol with 98% pentaerythritol comprises the following steps:
(1) Mixing water and the pentaerythritol crude, regulating the pH value to obtain a pentaerythritol solution I, and then heating and pressurizing for hydrolysis to obtain a hydrolysis material I;
(2) Decolorizing, press-filtering, crystallizing and press-filtering the hydrolysis material I obtained in the step (1) again to obtain a crystal I and a filtrate I, and drying the crystal I to obtain 98% pentaerythritol; wherein, the filtrate is recycled and reused, and returned to the step (1) to be mixed with water and pentaerythritol crude product for use;
(3) Mixing the crystal I obtained in the step (2) with a pentaerythritol crude product, regulating the pH value to obtain a pentaerythritol solution II, and heating and pressurizing to hydrolyze to obtain a hydrolysis material II;
(4) Decolorizing, press-filtering, crystallizing and press-filtering the hydrolysis material II obtained in the step (3) again to obtain a crystal II and a filtrate II; wherein, the second filtrate is recycled and reused, and returned to the step (3) to be mixed with the crude product of the first crystal and the pentaerythritol;
(5) And (3) drying the crystal II obtained in the step (4) to obtain 99% pentaerythritol.
In other specific embodiments, the preparation method for co-producing 99% pentaerythritol with 98% pentaerythritol comprises the following steps:
s1: mixing the filtrate I with the crude product of pentaerythritol, then placing the mixture into a dissolution kettle, adding methanesulfonic acid to adjust the pH of the solution, preparing to obtain pentaerythritol solution I, heating and pressurizing for hydrolysis to obtain hydrolysis material I;
s2: adding active carbon into the hydrolyzed material I, decoloring at normal pressure, press-filtering, removing carbon residues and colored impurities, cooling the mother solution, stirring, crystallizing, press-filtering to obtain crystal I and filtrate I, wherein the filtrate I returns to the first step for the next preparation; drying the first crystal to obtain 98% pentaerythritol;
s3: mixing the filtrate II with the obtained primary crystal and the pentaerythritol crude product, then placing the mixture into a dissolution kettle, adding methanesulfonic acid to adjust the pH of the solution, preparing a pentaerythritol solution II, heating and pressurizing for hydrolysis to obtain a hydrolysis material II;
s4: adding active carbon into the hydrolyzed material II, decoloring at normal pressure, press-filtering, removing carbon slag and colored impurities, cooling the mother liquor, stirring, crystallizing, and press-filtering to obtain filtrate II and crystal II, wherein the filtrate II returns to the step S1 for the next preparation;
s5: and drying the obtained crystal II to obtain a 99% pentaerythritol finished product.
The invention has the technical effects that:
1. in the industry, it is extremely difficult to increase the pentaerythritol yield to approximately 100%, such as above 98%. According to the pressurizing hydrolysis method of the methanesulfonic acid, according to the chemical properties of organic chemical ether, acetal and the like, under the conditions of acidity, high temperature and high pressure, chemical bonds such as ether bonds and the like can be broken, and the hydrolysis of dipentaerythritol (dipentaerythritol, tripentaerythritol and tetrapentaerythritol), the shrinkage ether, pentaerythritol formal and the like can be converted into pentaerythritol, so that more pentaerythritol can be recovered, and the overall yield of the pentaerythritol is improved.
2. The invention uses the methanesulfonic acid with high boiling point instead of the volatile one, has strong corrosiveness, affects the hydrolysis effect, has higher risks of formic acid and sulfuric acid, and has better safety and less loss;
3. according to the invention, the crude pentaerythritol product is directly hydrolyzed, and after crystallization, the crude pentaerythritol product is hydrolyzed, decolored and secondarily crystallized to purify the pentaerythritol product, so that the step of purifying the crude pentaerythritol product is omitted, and the cost is reduced;
4. according to the invention, the crystallization mother liquor in a specific step in the production flow is stored and is continuously used for the hydrolysis reaction of the raw materials in the next production flow, so that the use amount of methanesulfonic acid is reduced, and the production cost is reduced; meanwhile, the mother solution also contains pentaerythritol, and the pentaerythritol is stored and used for the next production flow, and the pentaerythritol circulates in the production flow without flowing out of the production flow, so that the loss of the pentaerythritol is greatly reduced and the overall yield of the pentaerythritol is greatly improved under the condition of repeated circulation use;
5. the invention uses the wooden activated carbon to decolorize by-products such as the shrinkage ether, the formal and the like, and the common coal activated carbon contains a large amount of sulfur, iron and other impurities, and the iron and organic matters can form a complex, so that the color of the complex is yellow, and the chromaticity of pentaerythritol products is influenced. The wood activated carbon has developed pores, good adsorption performance, high strength, easy regeneration, economy and durability, and can ensure that the chromaticity of pentaerythritol is within 30.
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present invention with reference to specific examples. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention.
Before the embodiments of the invention are explained in further detail, it is to be understood that the invention is not limited in its scope to the particular embodiments described below; it is also to be understood that the terminology used in the examples of the invention is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the invention.
Where numerical ranges are provided in the examples, it is understood that unless otherwise stated herein, both endpoints of each numerical range and any number between the two endpoints are significant both in the numerical range. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is worth noting that the raw materials used in the invention are all common commercial products, so the sources thereof are not particularly limited; the filtrate used in the step (1) is recycled to the step (1) after being obtained from the step (2).
Example 1
The crude pentaerythritol used in example 1 has the main ingredients shown in Table 1:
TABLE 1 crude pentaerythritol composition table
| Sequence number | Component (A) | Mass percent is percent |
| 1 | Monopentaerythritol | 85.13 |
| 2 | Dipentaerythritol | 3.96 |
| 3 | Tripentaerythritol | 0.87 |
| 4 | Moisture content | 9.75 |
| 5 | Impurity(s) | 0.29 |
For the crude pentaerythritol product of Table 1, the procedure was as follows.
(1) Mixing the filtrate I with the pentaerythritol crude according to the weight ratio of 3:1, then placing the mixture into a dissolution kettle, adding methanesulfonic acid to adjust the pH value of the solution to 2.2, preparing the pentaerythritol solution I, heating, pressurizing and hydrolyzing, wherein the pressure is 0.23Mpa, and the reaction temperature is 130 ℃ for 4 hours to obtain a hydrolyzed material I;
(2) Adding 150-mesh coconut shell powder active carbon accounting for 2.0% of the total amount of wet materials into the hydrolyzed material I, decoloring for 15min at normal pressure and 90 ℃, performing filter pressing, removing carbon residues and colored impurities, cooling the mother liquor to 30 ℃, stirring at a speed of 5r/min, crystallizing for 4h, and performing filter pressing to obtain crystal I and filtrate I, wherein the filtrate I returns to the first step for preparation and use next time; drying the first crystal to obtain 98% pentaerythritol with the composition shown in Table 2;
(3) Mixing the filtrate II with the obtained primary crystal and the pentaerythritol crude product according to the ratio of 6:1:1, then placing the mixture into a dissolution kettle, adding methanesulfonic acid to adjust the pH value of the solution to 2.5, preparing a pentaerythritol solution II, heating, pressurizing and hydrolyzing, wherein the pressure is 0.23Mpa, the reaction temperature is 130 ℃ and the time is 4 hours, and obtaining a hydrolyzed material II;
(4) Adding 150-mesh coconut shell powder active carbon accounting for 2.0% of the total amount of wet materials into the hydrolyzed material II, decoloring for 15min at normal pressure and 90 ℃, performing filter pressing, removing carbon residues and colored impurities, cooling the mother liquor to 30 ℃, stirring at a speed of 10r/min, crystallizing for 4h, and crystallizing at a stirring speed of 20r/min, wherein filtrate II and crystal II are obtained after filter pressing, and the filtrate II returns to the step (1) for the next preparation;
(5) The obtained crystal II is dried to obtain 99% pentaerythritol finished product, and the specific results are shown in Table 3.
The 98% pentaerythritol and 99% pentaerythritol obtained were tested, and the test results are shown in tables 2 and 3, respectively.
Table 2 table of 98% pentaerythritol quality
| Sequence number | Component (A) | Quality of |
| 1 | Monopentaerythritol | 98.01％ |
| 2 | Chromaticity of | 80 |
| 3 | Moisture content | 0.25％ |
| 4 | Ash content | 0.03％ |
| 5 | Others | 1.74％ |
| 6 | Average particle diameter | 40 mesh |
TABLE 3 99% pentaerythritol quality table
| Sequence number | Component (A) | Quality of |
| 1 | Monopentaerythritol | 99.71％ |
| 2 | Chromaticity of | 20 |
| 3 | Moisture content | 0.29％ |
| 4 | Ash content | 0.01％ |
| 5 | Average particle diameter | 80 mesh |
Example 2
The crude pentaerythritol used in example 2 has the main ingredients shown in Table 4:
TABLE 4 crude pentaerythritol composition Table
For the crude pentaerythritol product of Table 4, the procedure was as follows.
(1) Mixing the filtrate I with the pentaerythritol crude according to the weight ratio of 4:1, then placing the mixture into a dissolution kettle, adding methanesulfonic acid to adjust the pH value of the solution to 2.3, preparing the pentaerythritol solution I, heating, pressurizing and hydrolyzing, wherein the pressure is 0.3Mpa, and the reaction temperature is 140 ℃ for 4 hours to obtain a hydrolyzed material I;
(2) Adding 200-mesh wood powder active carbon accounting for 1.5% of the total amount of wet materials into the hydrolyzed material I, decoloring for 15min at the normal pressure of 95 ℃, press-filtering, removing carbon residues and colored impurities, cooling the mother liquor to 35 ℃, stirring at the speed of 15r/min, crystallizing for 5h, press-filtering to obtain crystal I and filtrate I, wherein the filtrate I returns to the first step for the next preparation; drying the first crystal to obtain 98% pentaerythritol with the composition shown in Table 5;
(3) Mixing the filtrate II with the obtained primary crystal and the pentaerythritol crude product according to the ratio of 6:1:1, then placing the mixture into a dissolution kettle, adding methanesulfonic acid to adjust the pH value of the solution to 2.8, heating, preparing to obtain pentaerythritol solution II, carrying out pressurized hydrolysis, wherein the pressure is 0.3Mpa, and the reaction temperature is 140 ℃ for 4 hours to obtain hydrolyzed material II;
(4) Adding 200-mesh wood powder active carbon accounting for 3.5% of the total amount of wet materials into the hydrolyzed material II, decoloring for 15min at the normal pressure of 95 ℃, press-filtering, removing carbon residues and colored impurities, cooling the mother liquor to 35 ℃, stirring at the speed of 25r/min, crystallizing for 5h, and crystallizing at the stirring speed of 22r/min, wherein filtrate II and crystal II are obtained after press-filtering, and the filtrate II is returned to the step (1) for the next preparation;
(5) The obtained crystal II is dried to obtain 99% pentaerythritol finished product, and the specific results are shown in Table 6.
The 98% pentaerythritol and 99% pentaerythritol obtained were tested, and the test results are shown in tables 5 and 6, respectively.
Table 5 shows the quality of 98% pentaerythritol
| Sequence number | Component (A) | Quality of |
| 1 | Monopentaerythritol | 98.34％ |
| 2 | Chromaticity of | 70 |
| 3 | Moisture content | 0.20％ |
| 4 | Ash content | 0.02％ |
| 5 | Others | 1.46％ |
| 6 | Average particle diameter | 85 mesh |
Table 6 99% pentaerythritol quality table
| Sequence number | Component (A) | Quality of |
| 1 | Monopentaerythritol | 99.83％ |
| 2 | Chromaticity of | 20 |
| 3 | Moisture content | 0.17％ |
| 4 | Ash content | 0.02％ |
| 5 | Average particle diameter | 150 mesh |
Example 3
The crude pentaerythritol used in example 3 has the main ingredients shown in Table 7:
TABLE 7 crude pentaerythritol composition table
| Sequence number | Component (A) | Mass percent is percent |
| 1 | Monopentaerythritol | 89.32 |
| 2 | Dipentaerythritol | 2.56 |
| 3 | Tripentaerythritol | 0.61 |
| 4 | Moisture content | 7.33 |
| 5 | Impurity(s) | 0.18 |
For the crude pentaerythritol product of Table 7, the procedure was as follows.
(1) Mixing the filtrate I with the pentaerythritol crude according to the weight ratio of 5:1, then placing the mixture into a dissolution kettle, adding methanesulfonic acid to adjust the pH value of the solution to 2.4, heating, preparing the pentaerythritol solution I, carrying out pressurized hydrolysis, wherein the pressure is 0.25Mpa, and the reaction temperature is 135 ℃ for 6 hours;
(2) Adding 100-mesh coconut shell powder active carbon accounting for 1.5% of the total amount of wet materials into the hydrolyzed material I, decoloring for 15min at the normal pressure of 100 ℃, performing filter pressing, removing carbon residues and colored impurities, cooling the mother liquor to 40 ℃, stirring at the speed of 13r/min, crystallizing for 6h, and performing filter pressing to obtain crystal I and filtrate I, wherein the filtrate I returns to the first step for the next preparation; drying the first crystal to obtain 98% pentaerythritol with the composition shown in Table 8;
(3) Preparing a pentaerythritol solution II: mixing the filtrate II with the obtained primary crystal and the pentaerythritol crude product according to the ratio of 6:1:1, then placing the mixture into a dissolution kettle, adding methanesulfonic acid to adjust the pH value of the solution to 2.9, heating, preparing to obtain pentaerythritol solution II, carrying out pressurized hydrolysis, wherein the pressure is 0.15Mpa, and the reaction temperature is 115 ℃ for 6 hours to obtain hydrolyzed material II;
(4) Adding 100-mesh coconut shell powder active carbon accounting for 3.5% of the total amount of wet materials into the hydrolyzed material II, decoloring for 15min at the normal pressure of 100 ℃, performing filter pressing, removing carbon residues and colored impurities, cooling the mother liquor to 40 ℃, stirring at the speed of 15r/min, crystallizing for 6h, and crystallizing at the stirring speed of 18r/min, wherein the filter liquor II returns to the step (1) for the next preparation;
(5) The obtained crystal II is dried to obtain 99% pentaerythritol finished product, and the specific results are shown in Table 9.
The 98% pentaerythritol and 99% pentaerythritol obtained were tested, and the test results are shown in tables 8 and 9, respectively.
Table 8 shows the quality of 98% pentaerythritol
| Sequence number | Component (A) | Quality of |
| 1 | Monopentaerythritol | 98.71％ |
| 2 | Chromaticity of | 60 |
| 3 | Moisture content | 0.12％ |
| 4 | Ash content | 0.01％ |
| 5 | Others | 1.17％ |
| 6 | Average particle diameter | 88 mesh |
Table 9 99% pentaerythritol quality table
| Sequence number | Component (A) | Quality of |
| 1 | Monopentaerythritol | 99.87％ |
| 2 | Chromaticity of | 20 |
| 3 | Moisture content | 0.13％ |
| 4 | Ash content | 0.01％ |
| 7 | Average particle diameter | 93 mesh of |
Example 4
The crude pentaerythritol used in example 4 has the main ingredients shown in Table 10.
TABLE 10 crude pentaerythritol compositions Table
| Sequence number | Component (A) | Mass percent is percent |
| 1 | Monopentaerythritol | 88.07 |
| 2 | Dipentaerythritol | 3.89 |
| 3 | Tripentaerythritol | 0.76 |
| 4 | Moisture content | 7.14 |
| 5 | Impurity(s) | 0.14 |
The procedure was as follows for the crude pentaerythritol product of Table 10.
(1) Mixing the filtrate I with the pentaerythritol crude according to the weight ratio of 3.5:1, then placing the mixture into a dissolution kettle, adding methanesulfonic acid to adjust the pH value of the solution to 2.5, heating, preparing the pentaerythritol solution I, carrying out pressurized hydrolysis, wherein the pressure is 0.20Mpa, and the reaction temperature is 125 ℃ for 5 hours;
(2) Adding 150-mesh coconut shell powder active carbon accounting for 1.5% of the total amount of wet materials into the hydrolyzed material I, decoloring for 15min at the normal pressure of 105 ℃, performing filter pressing, removing carbon residues and colored impurities, cooling the mother liquor to 45 ℃, stirring at the speed of 8r/min, crystallizing for 5h, and performing filter pressing to obtain crystal I and filtrate I, wherein the filtrate I returns to the first step for the next preparation; drying the first crystal to obtain 98% pentaerythritol with the composition shown in Table 11;
(3) Mixing the filtrate II with the obtained primary crystal and the pentaerythritol crude product according to the ratio of 6:1:1, then placing the mixture into a dissolution kettle, adding methanesulfonic acid to adjust the pH value of the solution to 2.8, heating, preparing to obtain pentaerythritol solution II, carrying out pressurized hydrolysis, wherein the pressure is 0.20Mpa, and the reaction temperature is 125 ℃ for 5 hours to obtain hydrolyzed material II;
(4) Adding 150-mesh coconut shell powder active carbon accounting for 2.5% of the total amount of wet materials into the hydrolyzed material II, decoloring for 15min at the normal pressure of 105 ℃, performing filter pressing, removing carbon residues and colored impurities, cooling the mother liquor to 45 ℃, stirring at the rate of 17r/min, crystallizing for 5h, and crystallizing at the stirring rate of 18r/min, wherein the filter liquor II returns to the step (1) for the next preparation;
(5) The obtained crystal II is dried to obtain 99% pentaerythritol finished product, and the specific results are shown in Table 12.
The 98% pentaerythritol and 99% pentaerythritol obtained were tested, and the test results are shown in tables 11 and 12, respectively.
Table 11 preparation of a 98% pentaerythritol quality table
| Sequence number | Component (A) | Quality of |
| 1 | Monopentaerythritol | 98.52％ |
| 2 | Chromaticity of | 70 |
| 3 | Moisture content | 0.15％ |
| 4 | Ash content | 0.02％ |
| 5 | Others | 1.33％ |
| 6 | Average particle diameter | 70 mesh |
Table 12 99% pentaerythritol quality table
Example 5
The crude pentaerythritol used in example 5 has the main ingredients shown in Table 13:
TABLE 13 crude pentaerythritol compositions Table
| Sequence number | Component (A) | Mass percent is percent |
| 1 | Monopentaerythritol | 85.16 |
| 2 | Dipentaerythritol | 4.01 |
| 3 | Tripentaerythritol | 0.59 |
| 4 | Moisture content | 10.08 |
| 5 | Impurity(s) | 0.16 |
The procedure was as follows for the crude pentaerythritol product of Table 13.
(1) Mixing the filtrate I with the pentaerythritol crude according to the weight ratio of 4.5:1, then placing the mixture into a dissolution kettle, adding methanesulfonic acid to adjust the pH value of the solution to 2.4, heating, preparing the pentaerythritol solution I, carrying out pressurized hydrolysis, wherein the pressure is 0.10Mpa, and the reaction temperature is 110 ℃ for 3 hours;
(2) Adding 200-mesh wood powder active carbon accounting for 1.0% of the total amount of wet materials into the hydrolyzed material I, decoloring for 15min at the normal pressure of 110 ℃, press-filtering, removing carbon residues and colored impurities, cooling the mother liquor to 50 ℃, stirring at the speed of 20r/min, crystallizing for 3h, press-filtering to obtain crystal I and filtrate I, wherein the filtrate I returns to the first step for the next preparation; drying the first crystal to obtain 98% pentaerythritol with the composition shown in Table 14;
(3) Mixing the filtrate II with the obtained primary crystal and the pentaerythritol crude product according to the ratio of 6:1:1, then placing the mixture into a dissolution kettle, adding methanesulfonic acid to adjust the pH value of the solution to 3.0, heating, preparing to obtain pentaerythritol solution II, carrying out pressurized hydrolysis, wherein the pressure is 0.10Mpa, and the reaction temperature is 110 ℃ for 3 hours to obtain hydrolyzed material II;
(4) Adding 200-mesh wood powder active carbon accounting for 2.0% of the total amount of wet materials into the hydrolyzed material II, decoloring for 15min at the normal pressure of 110 ℃, press-filtering, removing carbon residues and colored impurities, cooling the mother liquor to 50 ℃, stirring at the rate of 35r/min, crystallizing for 3h, crystallizing at the stirring rate of 20r/min, and press-filtering to obtain filtrate II and crystal II, wherein the filtrate II returns to the step (1) for the next preparation;
(5) The obtained crystal II is dried to obtain 99% pentaerythritol finished product, and the specific results are shown in Table 15.
The 98% pentaerythritol and 99% pentaerythritol obtained were tested, and the test results are shown in tables 14 and 15, respectively.
Table 14 table of 98% pentaerythritol quality
| Sequence number | Component (A) | Quality of |
| 1 | Monopentaerythritol | 98.59％ |
| 2 | Chromaticity of | 80 |
| 3 | Moisture content | 0.22％ |
| 4 | Ash content | 0.02％ |
| 5 | Others | 1.19％ |
| 6 | Average particle diameter | 190 mesh |
Table 15 99% pentaerythritol quality table
| Sequence number | Component (A) | Quality of |
| 1 | Monopentaerythritol | 99.25％ |
| 2 | Chromaticity of | 30 |
| 3 | Moisture content | 0.75％ |
| 4 | Ash content | 0.04％ |
| 5 | Average particle diameter | 200 mesh |
Example 6
The crude pentaerythritol used in example 6 has the main ingredients shown in Table 16:
TABLE 16 crude pentaerythritol composition Table
The procedure was as follows for the crude pentaerythritol product of Table 16.
(1) Mixing the filtrate I with the pentaerythritol crude according to the weight ratio of 3:1, then placing the mixture into a dissolution kettle, adding methanesulfonic acid to adjust the pH value of the solution to 2.4, heating, preparing the pentaerythritol solution I, carrying out pressurized hydrolysis, wherein the pressure is 0.15Mpa, and the reaction temperature is 120 ℃ for 4 hours;
(2) Adding 150-mesh wood powder active carbon accounting for 1.5% of the total amount of wet materials into the hydrolyzed material I, decoloring for 15min at the normal pressure of 110 ℃, press-filtering, removing carbon residues and colored impurities, cooling the mother liquor to 45 ℃, stirring at the speed of 9r/min, crystallizing for 5h, press-filtering to obtain crystal I and filtrate I, wherein the filtrate I returns to the first step for the next preparation; drying the first crystal to obtain 98% pentaerythritol with the composition shown in Table 17;
(3) Mixing the filtrate II with the obtained primary crystal and the pentaerythritol crude product according to the ratio of 6:1:1, then placing the mixture into a dissolution kettle, adding methanesulfonic acid to adjust the pH value of the solution to 2.8, heating, preparing to obtain pentaerythritol solution II, carrying out pressurized hydrolysis, wherein the pressure is 0.15Mpa, and the reaction temperature is 120 ℃ for 4 hours to obtain hydrolyzed material II;
(4) Adding 150-mesh wood powder active carbon accounting for 3.5% of the total amount of wet materials into the hydrolyzed material II, decoloring for 15min at the normal pressure of 110 ℃, press-filtering, removing carbon residues and colored impurities, cooling the mother liquor to 45 ℃, stirring at the rate of 11r/min, crystallizing for 5h, and crystallizing at the stirring rate of 22r/min, wherein filtrate II and crystal II are obtained after press-filtering, and the filtrate II returns to the step (1) for the next preparation;
(5) The obtained crystal II was dried to obtain 99% pentaerythritol finished product, and the specific results are shown in Table 18.
The 98% pentaerythritol and 99% pentaerythritol obtained were tested, and the test results are shown in tables 17 and 18, respectively.
Table 17 shows the quality of 98% pentaerythritol
| Sequence number | Component (A) | Quality of |
| 1 | Monopentaerythritol | 98.62％ |
| 2 | Chromaticity of | 90 |
| 3 | Moisture content | 0.25％ |
| 4 | Ash content | 0.03％ |
| 5 | Others | 1.13％ |
| 6 | Average particle diameter | 75 mesh |
Table 18 99% pentaerythritol quality table
| Sequence number | Component (A) | Quality of |
| 1 | Monopentaerythritol | 99.45％ |
| 2 | Chromaticity of | 20 |
| 3 | Moisture content | 0.55％ |
| 4 | Ash content | 0.03％ |
| 5 | Average particle diameter | 87 mesh(s) |
Comparative example 1
Comparative example 1 using the crude pentaerythritol product of example 1 (see table 1 for details of the specific ingredients), the catalyst was phosphoric acid, the specific procedure was as follows:
(1) Mixing the filtrate I with the pentaerythritol crude according to the weight ratio of 3:1, then placing the mixture into a dissolution kettle, adding phosphoric acid to adjust the pH value of the solution to 2.2, preparing the pentaerythritol solution I, heating, pressurizing and hydrolyzing, wherein the pressure is 0.23Mpa, and the reaction temperature is 130 ℃ for 4 hours to obtain a hydrolyzed material I;
(2) Adding 150-mesh coconut shell powder active carbon accounting for 2.0% of the total amount of wet materials into the hydrolyzed material I, decoloring for 15min at normal pressure and 90 ℃, performing filter pressing, removing carbon residues and colored impurities, cooling the mother liquor to 30 ℃, stirring at a speed of 5r/min, crystallizing for 4h, and performing filter pressing to obtain crystal I and filtrate I, wherein the filtrate I returns to the first step for preparation and use next time; drying the first crystal to obtain 98% pentaerythritol with the composition shown in Table 19;
(3) Mixing the filtrate II with the obtained primary crystal and the pentaerythritol crude product according to the ratio of 6:1:1, then placing the mixture into a dissolution kettle, adding phosphoric acid to adjust the pH value of the solution to 2.5, preparing a pentaerythritol solution II, heating, pressurizing and hydrolyzing, wherein the pressure is 0.23Mpa, and the reaction temperature is 130 ℃ for 4 hours to obtain a hydrolyzed material II;
(4) Adding 150-mesh coconut shell powder active carbon accounting for 2.0% of the total amount of wet materials into the hydrolyzed material II, decoloring for 15min at normal pressure and 90 ℃, performing filter pressing, removing carbon residues and colored impurities, cooling the mother liquor to 30 ℃, stirring at a speed of 10r/min, crystallizing for 4h, and crystallizing at a stirring speed of 20r/min, wherein filtrate II and crystal II are obtained after filter pressing, and the filtrate II returns to the step (1) for the next preparation;
(5) The obtained crystal II is dried to obtain 99% pentaerythritol finished product, and the specific results are shown in Table 20.
The 98% pentaerythritol and 99% pentaerythritol obtained were tested, and the test results are shown in tables 19 and 20, respectively.
Table 19 shows the quality of 98% pentaerythritol
| Sequence number | Component (A) | Quality of |
| 1 | Monopentaerythritol | 96.87％ |
| 2 | Chromaticity of | 100 |
| 3 | Moisture content | 0.44％ |
| 4 | Ash content | 0.14％ |
| 5 | Others | 2.69％ |
| 6 | Average particle diameter | 40 mesh |
Table 20 99% pentaerythritol quality table
Comparative example 2
Comparative example 2 using the crude pentaerythritol product of example 2 (see table 4 for details of the specific ingredients), the catalyst was phosphoric acid, the specific procedure was as follows:
(1) Mixing the filtrate I with the pentaerythritol crude according to the weight ratio of 4:1, then placing the mixture into a dissolution kettle, adding methanesulfonic acid to adjust the pH value of the solution to 2.3, preparing the pentaerythritol solution I, heating, pressurizing and hydrolyzing, wherein the pressure is 0.1Mpa, and the reaction temperature is 90 ℃ for 4 hours to obtain a hydrolyzed material I;
(2) Adding 200-mesh wood powder active carbon accounting for 1.5% of the total amount of wet materials into the hydrolyzed material I, decoloring for 15min at the normal pressure of 95 ℃, press-filtering, removing carbon residues and colored impurities, cooling the mother liquor to 35 ℃, stirring at the speed of 15r/min, crystallizing for 5h, press-filtering to obtain crystal I and filtrate I, wherein the filtrate I returns to the first step for the next preparation; drying the first crystal to obtain 98% pentaerythritol with the composition shown in Table 21;
(3) Mixing the filtrate II with the obtained primary crystal and the pentaerythritol crude product according to the ratio of 6:1:1, then placing the mixture into a dissolution kettle, adding methanesulfonic acid to adjust the pH value of the solution to 2.8, heating, preparing to obtain pentaerythritol solution II, carrying out pressurized hydrolysis, wherein the pressure is 0.1Mpa, and the reaction temperature is 90 ℃ for 4 hours to obtain hydrolyzed material II;
(4) Adding 200-mesh wood powder active carbon accounting for 3.5% of the total amount of wet materials into the hydrolyzed material II, decoloring for 15min at the normal pressure of 95 ℃, press-filtering, removing carbon residues and colored impurities, cooling the mother liquor to 35 ℃, stirring at the speed of 25r/min, crystallizing for 5h, and crystallizing at the stirring speed of 22r/min, wherein filtrate II and crystal II are obtained after press-filtering, and the filtrate II is returned to the step (1) for the next preparation;
(5) The obtained crystal II was dried to obtain 99% pentaerythritol finished product, and the specific results are shown in Table 22.
The 98% pentaerythritol and 99% pentaerythritol obtained were tested, and the test results are shown in tables 21 and 22, respectively.
Table 21 Table 98% pentaerythritol quality is obtained
| Sequence number | Component (A) | Quality of |
| 1 | Monopentaerythritol | 96.86％ |
| 2 | Chromaticity of | 100 |
| 3 | Moisture content | 0.37％ |
| 4 | Ash content | 0.15％ |
| 5 | Others | 2.77％ |
| 6 | Average particle diameter | 85 mesh |
Table 22 99% pentaerythritol quality table
| Sequence number | Component (A) | Quality of |
| 1 | Monopentaerythritol | 97.43％ |
| 2 | Chromaticity of | 60 |
| 3 | Moisture content | 0.29％ |
| 4 | Ash content | 0.08％ |
| 5 | Others | 2.28％ |
| 6 | Average particle diameter | 150 mesh |
Comparative example 3
Comparative example 3 using the crude pentaerythritol product of example 3 (see table 7 for details of the specific ingredients), the catalyst was phosphoric acid, the specific procedure was as follows:
(1) Mixing the filtrate I with the pentaerythritol crude according to the weight ratio of 5:1, then placing the mixture into a dissolution kettle, adding methanesulfonic acid to adjust the pH value of the solution to 3.5, heating, preparing the pentaerythritol solution I, carrying out pressurized hydrolysis, wherein the pressure is 0.25Mpa, and the reaction temperature is 135 ℃ for 6 hours;
(2) Adding 100-mesh coconut shell powder active carbon accounting for 1.5% of the total amount of wet materials into the hydrolyzed material I, decoloring for 15min at the normal pressure of 100 ℃, performing filter pressing, removing carbon residues and colored impurities, cooling the mother liquor to 40 ℃, stirring at the speed of 13r/min, crystallizing for 6h, and performing filter pressing to obtain crystal I and filtrate I, wherein the filtrate I returns to the first step for the next preparation; drying the first crystal to obtain 98% pentaerythritol with the composition shown in Table 23;
(3) Preparing a pentaerythritol solution II: mixing the filtrate II with the obtained primary crystal and the pentaerythritol crude product according to the ratio of 6:1:1, then placing the mixture into a dissolution kettle, adding methanesulfonic acid to adjust the pH value of the solution to 4.0, heating, preparing to obtain pentaerythritol solution II, carrying out pressurized hydrolysis, wherein the pressure is 0.15Mpa, and the reaction temperature is 115 ℃ for 6 hours to obtain hydrolyzed material II;
(4) Adding 100-mesh coconut shell powder active carbon accounting for 3.5% of the total amount of wet materials into the hydrolyzed material II, decoloring for 15min at the normal pressure of 100 ℃, performing filter pressing, removing carbon residues and colored impurities, cooling the mother liquor to 40 ℃, stirring at the speed of 15r/min, crystallizing for 6h, and crystallizing at the stirring speed of 18r/min, wherein the filter liquor II returns to the step (1) for the next preparation;
(5) The obtained crystal II is dried to obtain 99% pentaerythritol finished product, and the specific results are shown in Table 24.
The 98% pentaerythritol and 99% pentaerythritol obtained were tested, and the test results are shown in tables 23 and 24, respectively.
Table 23 table of 98% pentaerythritol quality
| Sequence number | Component (A) | Quality of |
| 1 | Monopentaerythritol | 96.51％ |
| 2 | Chromaticity of | 100 |
| 3 | Moisture content | 0.41％ |
| 4 | Ash content | 0.18％ |
| 5 | Others | 3.08％ |
| 6 | Average particle diameter | 88 mesh |
TABLE 24 preparation of 99% pentaerythritol quality table
From the results, it was found that the present invention was not achieved by using industrial pentaerythritol hydrolysis as a common acid phosphoric acid instead of methanesulfonic acid under the same conditions, both in terms of purity and chromaticity.
Finally, it should be noted that the above description is only for illustrating the technical solution of the present invention, and not for limiting the scope of the present invention, and that the simple modification and equivalent substitution of the technical solution of the present invention can be made by those skilled in the art without departing from the spirit and scope of the technical solution of the present invention.
Claims (10)
1. A preparation method for co-producing 99% pentaerythritol by 98% pentaerythritol is characterized by comprising the following steps: the method comprises the following steps:
(1) Mixing water and the pentaerythritol crude, adding methanesulfonic acid to adjust the pH value to obtain pentaerythritol solution I, and then heating and pressurizing to hydrolyze to obtain hydrolysis material I;
(2) Decolorizing, press-filtering, crystallizing and press-filtering the hydrolysis material I obtained in the step (1) again to obtain a crystal I and a filtrate I, and drying the crystal I to obtain 98% pentaerythritol;
(3) Mixing the crystal I obtained in the step (2) with a pentaerythritol crude product, adding methanesulfonic acid to adjust the pH to obtain a pentaerythritol solution II, and heating and pressurizing to hydrolyze to obtain a hydrolyzed material II;
(4) Decolorizing, press-filtering, crystallizing and press-filtering the hydrolysis material II obtained in the step (3) again to obtain a crystal II and a filtrate II;
(5) And (3) drying the crystal II obtained in the step (4) to obtain 99% pentaerythritol.
2. The method of manufacturing according to claim 1, characterized in that: the crude product of the pentaerythritol in the step (1) comprises 85-90% of monopentaerythritol, 3-5% of dipentaerythritol, 0.5-1% of tripentaerythritol and the balance of water.
3. The method of manufacturing according to claim 1, characterized in that: the pH of the pentaerythritol solution I in the step (1) is 2-2.5; the pH of the pentaerythritol solution II in the step (3) is 2.5-3.
4. The method of manufacturing according to claim 1, characterized in that: the weight ratio of the water to the pentaerythritol crude in the step (1) is 3-5:1; preferably 3:1.
5. The method of manufacturing according to claim 1, characterized in that: the temperature of the heating in the steps (1) and (3) is 110-140 ℃, the time is 3-6h, and the pressure of the pressurized hydrolysis is 0.1-0.3Mpa; the conditions for decoloring in the steps (2) and (4) are as follows: the temperature is 90-110 ℃ and the time is 15min, and the pressure is normal; the crystallization temperatures in the steps (2) and (4) are 30-50 ℃ and the crystallization time is 3-6h.
6. The method of manufacturing according to claim 1, characterized in that: the decolorization in the steps (2) and (4) is carried out by adding active carbon specifically, and the particle size is 100-200 meshes; the addition amount of the activated carbon in the step (2) is 1.0-2.0% of the total weight of the pentaerythritol crude, and the addition amount of the activated carbon in the step (2) is 2.0-4.0% of the total weight of the pentaerythritol crude.
7. The method of manufacturing according to claim 6, wherein: the activated carbon comprises coconut shell powder activated carbon and/or wood powder activated carbon.
8. The method of manufacturing according to claim 1, characterized in that: when the stirring rate of the crystallization in the step (4) is 5-10r/min, the crystal size is 40-80 meshes; when the stirring speed is 10-20r/min, the crystal size is 80-100 meshes; when the stirring speed is above 20r/min, the crystal size is 100-200 meshes.
9. The method of manufacturing according to claim 1, characterized in that: the filtrate I in the step (2) and the filtrate II in the step (4) are returned to the preparation process of the pentaerythritol solution I in the step (1) and/or the preparation process of the pentaerythritol solution II in the step (3) to replace water for use.
10. The method of manufacturing according to claim 9, wherein: the weight ratio of the filtrate II, the crystal I and the pentaerythritol crude in the step (3) is 5-7:1:1, preferably 6:1:1.
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