CN115926005A - Surface treating agent and preparation method and application thereof - Google Patents
Surface treating agent and preparation method and application thereof Download PDFInfo
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- CN115926005A CN115926005A CN202211660830.8A CN202211660830A CN115926005A CN 115926005 A CN115926005 A CN 115926005A CN 202211660830 A CN202211660830 A CN 202211660830A CN 115926005 A CN115926005 A CN 115926005A
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- Prior art keywords
- glyoxal
- dihydrogen phosphate
- sodium dihydrogen
- aqueous solution
- solution
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- 238000002360 preparation method Methods 0.000 title abstract description 10
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 claims abstract description 104
- 229940015043 glyoxal Drugs 0.000 claims abstract description 52
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims abstract description 35
- 235000019799 monosodium phosphate Nutrition 0.000 claims abstract description 35
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims abstract description 35
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims abstract description 32
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims abstract description 32
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims abstract description 32
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000007864 aqueous solution Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000000243 solution Substances 0.000 claims abstract description 17
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- 239000007787 solid Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000010790 dilution Methods 0.000 claims abstract description 6
- 239000012895 dilution Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000012756 surface treatment agent Substances 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 6
- 239000000047 product Substances 0.000 abstract description 32
- 238000004381 surface treatment Methods 0.000 abstract description 8
- 239000012043 crude product Substances 0.000 abstract description 3
- 230000008719 thickening Effects 0.000 description 9
- 150000002373 hemiacetals Chemical class 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 230000002035 prolonged effect Effects 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000006266 etherification reaction Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
- 150000001241 acetals Chemical class 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920003086 cellulose ether Polymers 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- -1 hydrogen ions Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910001410 inorganic ion Inorganic materials 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Abstract
A surface treating agent comprises a glyoxal aqueous solution and sodium dihydrogen phosphate dissolved in the glyoxal aqueous solution, wherein the concentration of the glyoxal aqueous solution is 4.0-5.0wt%, and the mass ratio of the sodium dihydrogen phosphate to the glyoxal aqueous solution is 16-16.4:974-1062, the pH value is 6.8-7.2, and the preparation method comprises the following steps: 1) Taking a commercially available glyoxal aqueous solution and solid sodium dihydrogen phosphate according to a certain proportion; 2) Adding desalted water into commercially available glyoxal aqueous solution for primary dilution; 3) Adding solid sodium dihydrogen phosphate, and stirring until the solid sodium dihydrogen phosphate is completely dissolved; 4) Adjusting the pH value to 6.8-7.2; 5) Adding desalted water for second dilution until the concentration of the glyoxal water solution is 4.0-5.0wt%. The method is used for surface treatment of the hydroxypropyl methyl cellulose crude product, reduces the surface treatment cost, adjusts the viscosity-rising time of the hydroxypropyl methyl cellulose finished product, and in addition, the quality of the treated product is kept stable within three months, thereby meeting the actual requirements of customers.
Description
Technical Field
The invention relates to the field of chemical industry, and particularly relates to a surface treating agent, and a preparation method and application thereof.
Background
When a chemical enterprise produces hydroxypropyl methyl cellulose (HPMC), cellulose is used as a raw material, alkalization and etherification reaction are carried out to obtain product powder (wet), and the product powder (wet) is washed, granulated, dried, crushed and sieved to obtain a product for sale.
Generally, the powder (wet) of the product obtained after the alkalization etherification reaction needs to be sprayed with glyoxal solution for surface treatment so as to prolong the sticking time of the product in water. However, glyoxal is expensive, which is not favorable for enterprises to reduce production cost.
Therefore, how to reduce the cost of the HPMC surface treatment process is an urgent problem to be solved by those skilled in the art.
Disclosure of Invention
One of the purposes of the invention is to provide a surface treating agent for surface treating a crude hydroxypropyl methyl cellulose product, reduce the surface treatment cost, adjust the tack-up time of the finished hydroxypropyl methyl cellulose product, and keep the quality of the treated product stable for three months to meet the actual requirements of customers.
The invention also aims to provide the preparation method of the surface treating agent, which has simple and convenient preparation process and meets the actual requirements of product manufacturers.
The technical scheme for realizing one purpose of the invention is as follows: a surface treating agent comprises a glyoxal aqueous solution and sodium dihydrogen phosphate dissolved in the glyoxal aqueous solution, wherein the concentration of the glyoxal aqueous solution is 4.0-5.0wt%, and the mass ratio of the sodium dihydrogen phosphate to the glyoxal aqueous solution is 16-16.4:974-1062 and its pH value is 6.8-7.2.
Preferably, the concentration of the glyoxal aqueous solution is 4.5wt%, and the mass-volume ratio of the sodium dihydrogen phosphate to the glyoxal aqueous solution is 16.4:1054 or 16:974 or 16:1062, pH 7.
Preferably, the pH is adjusted by the addition of sodium hydroxide.
The second technical scheme for realizing the purpose of the invention is as follows: the preparation method of any one of the above surface treatment agents comprises the following steps:
1) Taking a commercially available glyoxal aqueous solution and solid sodium dihydrogen phosphate according to a certain proportion;
2) Adding desalted water into commercially available glyoxal aqueous solution for primary dilution;
3) Adding solid sodium dihydrogen phosphate, and stirring until the solid sodium dihydrogen phosphate is completely dissolved;
4) Adjusting the pH value to 6.8-7.2;
5) Adding desalted water for second dilution until the concentration of the glyoxal water solution is 4.0-5.0wt%.
Further, the concentration of the commercially available glyoxal aqueous solution of the step 1) is 40wt%, and the solid sodium dihydrogen phosphate is powdered sodium dihydrogen phosphate.
Preferably, the pH value is adjusted by adding caustic soda flakes in the step 4).
The invention also claims the use of any of the above surface treatment agents for treating a hydroxypropyl methylcellulose raw product.
Further, the treatment is carried out by spraying or sprinkling on the surface of the hydroxypropyl methyl cellulose crude product, and the mass ratio of glyoxal in the sprayed or sprinkled surface treatment agent to the hydroxypropyl methyl cellulose crude product is 20-24:1000, the water content of the hydroxypropyl methyl cellulose is 3.5-10wt%.
Adopt above-mentioned technical scheme to have following beneficial effect:
1. the surface treating agent simultaneously contains glyoxal and sodium dihydrogen phosphate, wherein the glyoxal reacts with two free hydroxyl groups on the HPMC to form hemiacetal, so that the HPMC is moderately crosslinked, and the crosslinked product is insoluble in water but has better dispersing capacity in water. In the hydration stage (during dispersion in water), there is only a small amount of swelling, and at the same time, the hemiacetal structure starts to hydrolyze at a steady rate until the crosslinking member is broken, the molecular chains are uncrosslinked, the HPMC is rapidly dissolved, and the viscosity is sharply increased, however, too high or too low pH causes the hemiacetal to change into acetal, so that irreversible crosslinking occurs, resulting in complete insolubility of HPMC. The sodium dihydrogen phosphate mainly provides hydrogen ions to catalyze the reaction of the glyoxal and two free hydroxyl groups on the HPMC to become hemiacetal, so that the sticking time of the hydroxypropyl methyl cellulose after treatment can be effectively prolonged. The concentration of the glyoxal is controlled to be 4.0-5.0wt%, so that the sticking time of the HPMC is in a reasonable range, if the concentration is too low, the sticking time of the product is too short to meet the use requirement of a customer, and if the concentration is too high, the sticking time is too long, the use requirement of the customer can not be met, and the cost is high. Controlling the mass ratio of sodium dihydrogen phosphate to glyoxal water solution to be 16-16.4:974-1062, to avoid bringing more inorganic ions due to excessive sodium dihydrogen phosphate, and to avoid too high ash content in the product, which can not play a role in catalysis if the sodium dihydrogen phosphate is too low. The method can realize the purpose of controlling the sticking start time of the hydroxypropyl methyl cellulose by adjusting the proportion of the glyoxal and the hydroxypropyl methyl cellulose, for example, the content of the sodium dihydrogen phosphate is improved by reducing the content of the glyoxal, the dosage of the surface treating agent is reduced on the basis of meeting the requirement of customers for the long sticking start time of the HPMC, meanwhile, the cheap sodium dihydrogen phosphate replaces part of expensive glyoxal, and the unit production cost of the hydroxypropyl methyl cellulose can be reduced to a certain degree on the basis of meeting the actual requirement of the customers. In addition, sodium dihydrogen phosphate contained in the treating agent can also effectively slow down viscosity reduction of cellulose ether caused by oxidation of residual glyoxal into acid, so that the treated hydroxypropyl methyl cellulose product can keep stable viscosity-rising time, namely stable quality, within three months, and the competitiveness of the hydroxypropyl methyl cellulose product is further improved.
2. According to the preparation method of the surface treating agent, the commercially available glyoxal aqueous solution (with higher concentration) is firstly diluted by desalted water for the first time, and then solid sodium dihydrogen phosphate is added, so that the dissolving efficiency and effect of the sodium dihydrogen phosphate can be effectively improved. Adjusting pH to 6.8-7.2, and adding desalted water until the concentration of glyoxal is 4.0-5.0wt.
Through tests and production verification of an applicant, the hydroxypropyl methyl cellulose product obtained by the surface treatment agent provided by the invention has no change in the viscosity-rising time after being placed for three months, and the quality of the hydroxypropyl methyl cellulose product is proved to be stable for a long time.
The following description will be further described with reference to specific embodiments.
Detailed Description
In the invention, the aqueous solution of glyoxal is a commercial product with the concentration of 40wt%, the sodium dihydrogen phosphate is a commercial powder, the sodium dihydrogen phosphate is industrial pure, the caustic soda flakes are commercial products, the sodium dihydrogen phosphate is industrial pure, and the hydroxypropyl methyl cellulose is produced by the applicant.
Example 1
Preparation of surface treating agent
1) Adding 812kg of desalted water into a glyoxal solution tank;
2) Adding 162kg of glyoxal water solution into the glyoxal solution tank, and carrying out air mixing for 5min;
3) Dissolving 16.4kg solid sodium dihydrogen phosphate with 80kg desalted water, stirring until the solid is completely dissolved, observing whether the solution is transparent and has no impurities, adding the dissolved solution into a glyoxal solution tank, and air-mixing for 5min;
4) Adding 7-8.5kg of caustic soda flakes (dissolved by desalted water and then added), and adjusting the pH value to 6.8-7.2;
5) And after the pH value is qualified, adding desalted water to dilute the solution until the total mass of the solution is 2800kg, and then carrying out air mixing for 15min.
Specific addition amounts are shown in table 1:
TABLE 1
Spraying a surface treatment agent into the coarse products obtained by centrifugation after the alkalization process of different batches of production lines, sampling and detecting, wherein the specific data are shown in table 2:
TABLE 2
The same batch of the product only added with glyoxal as a surface treatment agent has the average thickening time of 6.98min and the maximum thickening time of 7.6min according to the same addition proportion.
The data show that: under the condition of not increasing the dosage of glyoxal, the surface treatment agent is adopted to carry out surface treatment on the product, and the thickening time is obviously prolonged.
Example 2
The preparation method of the surface treating agent is the same as that of example 1, and the specific addition amounts are shown in table 3:
TABLE 3
Spraying a surface treatment agent into the coarse products obtained by centrifugation after the alkalization process of different batches of production lines, sampling and detecting, wherein the specific data are shown in Table 4:
TABLE 4
The product which is added with only glyoxal as a surface treatment agent in the same batch has the average thickening time of 5.7min and the maximum thickening time of 6.7min according to the same adding proportion.
The data show that: under the condition of not increasing the dosage of glyoxal, the surface treatment agent is adopted to carry out surface treatment on the product, and the thickening time is obviously prolonged.
Example 3
The surface-treated hydroxypropylmethylcellulose product of example 1 was stored for a certain period of time according to the prescribed conditions, and then the thickening time was measured, as shown in table 5:
TABLE 5
Only glyoxal is added to the product serving as the surface treatment agent in the same batch, the maximum thickening time is increased by 2.6min after the product is placed for one month, and the maximum thickening time is increased by 4min after the product is placed for two months. The data show that: the surface treatment agent provided by the invention is used for surface treatment of products, and the quality stability of the products can be remarkably improved.
Claims (8)
1. The surface treating agent is characterized by comprising a glyoxal aqueous solution and sodium dihydrogen phosphate dissolved in the glyoxal aqueous solution, wherein the concentration of the glyoxal aqueous solution is 4.0-5.0wt%, and the mass ratio of the sodium dihydrogen phosphate to the glyoxal aqueous solution is 16-16.4:974-1062, and its pH value is 6.8-7.2.
2. The surface treatment agent according to claim 1, wherein the concentration of the aqueous glyoxal solution is 4.5wt%, and the mass-to-volume ratio of the sodium dihydrogen phosphate to the aqueous glyoxal solution is 16.4:1054 or 16:974 or 16:1062, pH 7.
3. The surface treating agent according to claim 1 or 2, characterized in that the pH is adjusted by adding sodium hydroxide.
4. A method for producing the surface treating agent according to any one of claims 1 to 3, characterized by comprising the steps of:
1) Taking a commercially available glyoxal aqueous solution and solid sodium dihydrogen phosphate according to a certain proportion;
2) Adding desalted water into commercially available glyoxal aqueous solution for primary dilution;
3) Adding solid sodium dihydrogen phosphate, and stirring until the solid sodium dihydrogen phosphate is completely dissolved;
4) Adjusting the pH value to 6.8-7.2;
5) Adding desalted water for second dilution until the concentration of the glyoxal water solution is 4.0-5.0wt%.
5. The method according to claim 4, wherein the concentration of the commercially available aqueous glyoxal solution of step 1) is 40wt%, and the solid sodium dihydrogen phosphate is powdered sodium dihydrogen phosphate.
6. The method according to claim 4, wherein the pH of the solution is adjusted by adding caustic soda flakes in the step 4).
7. Use of the surface treatment agent according to any one of claims 1 to 3 for the treatment of a hydroxypropyl methylcellulose raw product.
8. The use according to claim 7, wherein the treatment is sprayed or sprinkled on the surface of the hydroxypropyl methylcellulose raw product, the mass ratio of glyoxal to hydroxypropyl methylcellulose raw product in the sprayed or sprinkled surface treatment agent being 20-24:1000, the water content of the hydroxypropyl methyl cellulose is 3.5-10wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211660830.8A CN115926005A (en) | 2022-12-23 | 2022-12-23 | Surface treating agent and preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211660830.8A CN115926005A (en) | 2022-12-23 | 2022-12-23 | Surface treating agent and preparation method and application thereof |
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| Publication Number | Publication Date |
|---|---|
| CN115926005A true CN115926005A (en) | 2023-04-07 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202211660830.8A Pending CN115926005A (en) | 2022-12-23 | 2022-12-23 | Surface treating agent and preparation method and application thereof |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1421462A (en) * | 2001-11-28 | 2003-06-04 | 沃尔弗纤维素有限责任两合公司 | Delayed dissolved cellulose ether and producing process thereof |
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2022
- 2022-12-23 CN CN202211660830.8A patent/CN115926005A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1421462A (en) * | 2001-11-28 | 2003-06-04 | 沃尔弗纤维素有限责任两合公司 | Delayed dissolved cellulose ether and producing process thereof |
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