CN113884405A - Quantitative test method for characterizing pulp etherification reaction performance - Google Patents
Quantitative test method for characterizing pulp etherification reaction performance Download PDFInfo
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- CN113884405A CN113884405A CN202111136759.9A CN202111136759A CN113884405A CN 113884405 A CN113884405 A CN 113884405A CN 202111136759 A CN202111136759 A CN 202111136759A CN 113884405 A CN113884405 A CN 113884405A
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- pulp
- cellulose ether
- test method
- etherification reaction
- cellulose
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- 238000006266 etherification reaction Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000012113 quantitative test Methods 0.000 title claims abstract description 10
- 229920003086 cellulose ether Polymers 0.000 claims abstract description 60
- 239000007864 aqueous solution Substances 0.000 claims description 20
- 229920002678 cellulose Polymers 0.000 claims description 19
- 239000001913 cellulose Substances 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 13
- 229920000742 Cotton Polymers 0.000 claims description 9
- 238000000967 suction filtration Methods 0.000 claims description 9
- 238000006116 polymerization reaction Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 229920001131 Pulp (paper) Polymers 0.000 claims description 5
- 238000010998 test method Methods 0.000 claims description 5
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 4
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 4
- 241001330002 Bambuseae Species 0.000 claims description 4
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 4
- 239000011425 bamboo Substances 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000011158 quantitative evaluation Methods 0.000 abstract description 3
- 239000012153 distilled water Substances 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005034 decoration Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 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
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention provides a quantitative test method for characterizing the pulp etherification reaction performance, belonging to the technical field of cellulose ether production. According to the invention, by a quantitative test method, the yield A of the cellulose ether is firstly obtained, the percentage B of the unreacted pulp in the cellulose ether is further obtained, and the proportion of the non-etherified pulp in the pulp is measured to be C-BxA, so that the etherification performance of the pulp is reflected. The method can quickly and effectively carry out quantitative evaluation on the etherification performance of the pulp, thereby optimizing and selecting excellent pulp for production.
Description
Technical Field
The invention relates to the technical field of cellulose ether production, in particular to a quantitative test method for characterizing pulp etherification reaction performance.
Background
The traditional cellulose ether production process is as follows: the pulp is alkalized by sodium hydroxide under certain conditions to generate sodium cellulose, etherified by an etherifying agent, and reacted under certain conditions to generate cellulose ether, wherein the pulp is prepared from the following raw materials in parts by weight: the etherification reaction performances of cotton pulp, wood pulp, bamboo pulp and the like are different, and the etherification reaction performances of different product specifications of the cotton pulp are also different. What is specifically the amount of etherification that occurs after the pulp has undergone an etherification reaction? How much unreacted cellulose filaments remain? Currently, there is no specific method to quantitatively test this index. If the amount of the unreacted pulp is too large, the cellulose ether product contains too many water-insoluble cellulose filaments, which seriously affects the application of the product in the daily chemical industry. How to obtain a method for quickly and conveniently testing the etherification reaction performance of the pulp is a technical problem which is urgently needed to be solved at present.
Disclosure of Invention
The invention aims to provide a quantitative test method for characterizing the etherification reaction performance of pulp, which can quickly and effectively carry out quantitative evaluation on the etherification performance of the pulp so as to select excellent pulp for production.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a quantitative test method for characterizing the pulp etherification reaction performance, which comprises the following steps:
1) generating cellulose ether after pulp etherification reaction, wherein the yield of the cellulose ether is as follows: a-cellulose ether yield/pulp input;
2) and (2) carrying out suction filtration on the cellulose ether aqueous solution in a container to obtain a container with insoluble cellulose filaments, drying and weighing, wherein the percentage of the unreacted pulp in the cellulose ether is as follows: b ═ (N1-N0)/M;
3) the proportion of the non-etherified pulp in the pulp is as follows: c ═ B × a;
wherein M is the weight of the weighed cellulose ether, g; n0 is the dry weight of the container, g; n1 is the weight of the container with insoluble cellulose filaments, g.
Further, the pulp is one or more of cotton pulp, wood pulp and bamboo pulp.
Further, the polymerization degree of the pulp is 1040-2650.
Further, the mass concentration of the cellulose ether aqueous solution is 1-2%.
Further, the cellulose ether aqueous solution needs to be stirred before suction filtration, the rotating speed of stirring is 400-600 r/min, and the stirring time is 1-2 hours.
Further, the drying temperature is 130-140 ℃, and the drying time is 1-2 h.
The invention has the beneficial effects that:
in the production process of cellulose ether, the test method provided by the invention can effectively screen out high-quality pulp raw materials: the pulp has good etherification reaction performance, and the finally produced cellulose ether product has low content of insoluble cellulose filaments, thereby effectively meeting the requirements of clients in the daily chemical industry.
Detailed Description
The invention provides a quantitative test method for characterizing the pulp etherification reaction performance, which comprises the following steps:
1) generating cellulose ether after pulp etherification reaction, wherein the yield of the cellulose ether is as follows: a-cellulose ether yield/pulp input;
2) and (2) carrying out suction filtration on the cellulose ether aqueous solution in a container to obtain a container with insoluble cellulose filaments, drying and weighing, wherein the percentage of the unreacted pulp in the cellulose ether is as follows: b ═ (N1-N0)/M;
3) the proportion of the non-etherified pulp in the pulp is as follows: c ═ B × a;
wherein M is the weight of the weighed cellulose ether, g; n0 is the dry weight of the container, g; n1 is the weight of the container with insoluble cellulose filaments, g.
In the invention, the pulp is one or more of cotton pulp, wood pulp and bamboo pulp, and preferably cotton pulp.
In the present invention, the degree of polymerization of the pulp is 1040 to 2650, preferably 2550 to 2623, and more preferably 2600.
In the invention, the mass concentration of the cellulose ether aqueous solution is 1-2%, preferably 1.5%.
In the invention, the cellulose ether aqueous solution is stirred before suction filtration, the stirring speed is 400-600 r/min, and the stirring time is 1-2 h; preferably, the stirring speed is 450-550 r/min, and the stirring time is 1.5-2 h; more preferably, the rotation speed of stirring is 500r/min, and the stirring time is 1.5 h.
In the invention, the drying temperature is 130-140 ℃, and the drying time is 1-2 h; preferably, the drying temperature is 132-138 ℃, and the drying time is 1.5-2 h; further preferably, the drying temperature is 135 ℃, and the drying time is 1.5 h.
In the present invention, the container is preferably a sand-core crucible.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
The cotton pulp with the polymerization degree of 2600 is used as a raw material to produce a cellulose ether finished product. And calculating the yield of the cellulose ether according to the input amount and the output amount. A is cellulose ether yield/pulp input amount is 2.15;
weighing 2.350g of cellulose ether sample, adding the weighed sample into a 250ml glass beaker, adding 232.650g of distilled water to prepare a 1% cellulose ether aqueous solution, placing the cellulose ether aqueous solution on a magnetic stirrer to stir at the rotating speed of 500r/min until the sample is fully dissolved, then washing the sample, placing a sand core crucible on a filter flask, starting a vacuum pump, slowly pouring the cellulose ether aqueous solution into the sand core crucible to carry out suction filtration, and then washing the beaker with a large amount of distilled water until no cellulose exists on the wall of the glass beaker;
placing the sand core crucible with the insoluble cellulose filaments in a 135 ℃ oven for drying for 1.5 hours until the weight is constant, wherein the weighed weight is 23.630g, and the amount of the insoluble cellulose filaments is 0.050 g: i.e. the weight of pulp not subjected to etherification; calculating the percentage B of unreacted pulp in the cellulose ether to be 0.050/2.350 to be 2.13 percent according to the weight of the cellulose ether weighed when preparing the aqueous solution;
the yield of the first step of etherification reaction is 2.15, namely the proportion of the pulp which is not subjected to etherification reaction in the pulp is indirectly calculated to be 4.58%.
Example 2
The cotton pulp with the polymerization degree of 2623 is used as a raw material to produce a cellulose ether finished product. And calculating the yield of the cellulose ether according to the input amount and the output amount. A is cellulose ether yield/pulp input 2.07;
weighing 2.235g of a cellulose ether sample, adding the sample into a 250ml glass beaker, adding 221.265g of distilled water to prepare a 1% cellulose ether aqueous solution, placing the cellulose ether aqueous solution on a magnetic stirrer to stir at the rotating speed of 550r/min until the sample is fully dissolved, then washing the sample, placing a sand core crucible on a suction bottle, starting a vacuum pump, slowly pouring the cellulose ether aqueous solution into the sand core crucible to carry out suction filtration, and then washing the beaker with a large amount of distilled water until no cellulose exists on the wall of the glass beaker;
placing the sand core crucible with the insoluble cellulose filaments in an oven at 140 ℃ for drying for 2 hours until the weight is constant, wherein the weight is 23.356g, and the amount of the insoluble cellulose filaments is 0.006 g: i.e. the weight of pulp not subjected to etherification; calculating the percentage B of unreacted pulp in the cellulose ether to be 0.006/2.235 to be 0.27 percent according to the weight of the cellulose ether weighed when preparing the aqueous solution;
the yield of the first step of etherification reaction is 2.07, namely the proportion of the pulp which is not subjected to etherification reaction in the pulp is indirectly calculated to be 0.56 percent.
Example 3
The wood pulp with the polymerization degree of 1040 is used as a raw material to produce a cellulose ether finished product. And calculating the yield of the cellulose ether according to the input amount and the output amount. A is 2.00 cellulose ether yield/pulp input;
weighing 2.285g of cellulose ether sample, adding the weighed sample into a 250ml glass beaker, adding 226.215g of distilled water to prepare a 1% cellulose ether aqueous solution, placing the cellulose ether aqueous solution on a magnetic stirrer to stir at the rotating speed of 550r/min until the sample is fully dissolved, then washing the sample, placing a sand core crucible on a filter flask, starting a vacuum pump, slowly pouring the cellulose ether aqueous solution into the sand core crucible to carry out suction filtration, and then washing the beaker with a large amount of distilled water until no cellulose exists on the wall of the glass beaker;
placing the sand core crucible with the insoluble cellulose filaments in an oven at 140 ℃ for drying for 2 hours until the weight is constant, wherein the weighed weight is 23.338g, and the amount of the insoluble cellulose filaments is 0.063 g: i.e. the weight of pulp not subjected to etherification; calculating the percentage B of unreacted pulp in the cellulose ether to be 0.063/2.285 to be 2.8 percent according to the weight of the cellulose ether weighed when preparing the aqueous solution;
the yield of the first step of etherification reaction is 2.00, namely the proportion of the pulp which is not subjected to etherification reaction in the pulp can be indirectly calculated to be 5.6 percent.
The above embodiments show that the invention provides a quantitative test method for characterizing the etherification reaction performance of pulp, and the method can quickly and effectively carry out quantitative evaluation on the etherification performance of the pulp, so that excellent cotton pulp is selected for production.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (6)
1. The quantitative test method for characterizing the pulp etherification reaction performance is characterized by comprising the following steps of:
1) generating cellulose ether after pulp etherification reaction, wherein the yield of the cellulose ether is as follows: a-cellulose ether yield/pulp input;
2) and (2) carrying out suction filtration on the cellulose ether aqueous solution in a container to obtain a container with insoluble cellulose filaments, drying and weighing, wherein the percentage of the unreacted pulp in the cellulose ether is as follows: b ═ (N1-N0)/M;
3) the proportion of the non-etherified pulp in the pulp is as follows: c ═ B × a;
wherein M is the weight of the weighed cellulose ether, g; n0 is the dry weight of the container, g; n1 is the weight of the container with insoluble cellulose filaments, g.
2. The test method according to claim 1, wherein the pulp is one or more of cotton pulp, wood pulp, and bamboo pulp.
3. The method according to claim 2, wherein the degree of polymerization of the pulp is 1040 to 2650.
4. The test method according to claim 3, wherein the mass concentration of the aqueous cellulose ether solution is 1 to 2%.
5. The test method as claimed in any one of claims 1 to 4, wherein the cellulose ether aqueous solution is further stirred before suction filtration, the rotation speed of the stirring is 400 to 600r/min, and the stirring time is 1 to 2 hours.
6. The test method according to claim 5, wherein the drying temperature is 130-140 ℃ and the drying time is 1-2 h.
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| CN202111136759.9A CN113884405A (en) | 2021-09-27 | 2021-09-27 | Quantitative test method for characterizing pulp etherification reaction performance |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111136759.9A CN113884405A (en) | 2021-09-27 | 2021-09-27 | Quantitative test method for characterizing pulp etherification reaction performance |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102101891A (en) * | 2011-03-31 | 2011-06-22 | 河北吉藁化纤有限责任公司 | Cellulose ether and preparation method thereof |
| CN102967622A (en) * | 2011-09-02 | 2013-03-13 | 南通醋酸纤维有限公司 | Method and apparatus for evaluating cellulose pulp reaction performance |
| CN104897512A (en) * | 2015-05-28 | 2015-09-09 | 山东黄金矿业(莱州)有限公司精炼厂 | Rapid analysis method for acid insoluble substances in cyanide gold slime |
| CN106979929A (en) * | 2016-01-19 | 2017-07-25 | 中国制浆造纸研究院 | A kind of method of quick measure dissolving pulp reactivity worth |
| PL431574A1 (en) * | 2019-10-23 | 2020-03-09 | Instytut Techniki Budowlanej | Method of determining polymer microfibres content in cement composites |
-
2021
- 2021-09-27 CN CN202111136759.9A patent/CN113884405A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102101891A (en) * | 2011-03-31 | 2011-06-22 | 河北吉藁化纤有限责任公司 | Cellulose ether and preparation method thereof |
| CN102967622A (en) * | 2011-09-02 | 2013-03-13 | 南通醋酸纤维有限公司 | Method and apparatus for evaluating cellulose pulp reaction performance |
| CN104897512A (en) * | 2015-05-28 | 2015-09-09 | 山东黄金矿业(莱州)有限公司精炼厂 | Rapid analysis method for acid insoluble substances in cyanide gold slime |
| CN106979929A (en) * | 2016-01-19 | 2017-07-25 | 中国制浆造纸研究院 | A kind of method of quick measure dissolving pulp reactivity worth |
| PL431574A1 (en) * | 2019-10-23 | 2020-03-09 | Instytut Techniki Budowlanej | Method of determining polymer microfibres content in cement composites |
Non-Patent Citations (2)
| Title |
|---|
| 严瑞瑄: "《水溶性高分子》", 30 June 1998, 化学工业出版社, pages: 443 * |
| 梅自强: "《纺织辞典》", 中国纺织出版社, pages: 589 * |
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