CN112442892A - Method for catalytically hydrolyzing polyacrylonitrile material under acidic condition - Google Patents
Method for catalytically hydrolyzing polyacrylonitrile material under acidic condition Download PDFInfo
- Publication number
- CN112442892A CN112442892A CN202011205465.2A CN202011205465A CN112442892A CN 112442892 A CN112442892 A CN 112442892A CN 202011205465 A CN202011205465 A CN 202011205465A CN 112442892 A CN112442892 A CN 112442892A
- Authority
- CN
- China
- Prior art keywords
- pan
- acidic
- catalyst
- mixed solution
- acidic condition
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/55—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/13—Ammonium halides or halides of elements of Groups 1 or 11 of the Periodic System
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/155—Halides of elements of Groups 2 or 12 of the Periodic System
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/55—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
- D06M11/56—Sulfates or thiosulfates other than of elements of Groups 3 or 13 of the Periodic System
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
- D06M11/64—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with nitrogen oxides; with oxyacids of nitrogen or their salts
- D06M11/65—Salts of oxyacids of nitrogen
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
- D06M2101/28—Acrylonitrile; Methacrylonitrile
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Abstract
The invention relates to a method for catalyzing and hydrolyzing a polyacrylonitrile material under an acidic condition, belonging to the field of functional polymer materials. Adding a catalyst into the acidic solution to obtain a mixed solution, and heating to 60-130 ℃; and adding a PAN material into the mixed solution, reacting for 0.5-6 h, taking out the material after the reaction is finished, and washing to be neutral to obtain the PAN-COOH fiber. According to the method, the catalyst is added into the reaction solution, so that the concentration of hydrogen ions in the reaction solution is reduced, and the hydrolysis rate of the PAN material in a low-concentration acidic solution is increased.
Description
Technical Field
The invention relates to a method for catalytically hydrolyzing a Polyacrylonitrile (PAN) material under an acidic condition, in particular to a method for preparing a high-strength carboxylic acid type functional material by adding a catalyst into a reaction liquid to improve the hydrolysis rate of the PAN material in a low-concentration acid solution, and belongs to the field of functional polymer materials.
Background
The carboxyl group (-COOH) serves as a functional group, which can impart various effects to the material. In the field of air purification, the material containing carboxyl can effectively remove alkaline harmful gas in the air and purify the living environment. In the field of sewage treatment, a material containing carboxyl can adsorb heavy metal ions in water through ion exchange to treat industrial wastewater. In the field of new materials, materials containing carboxyl are used as substrates, functional compounds containing amino or other groups are grafted, and various functional materials can be prepared.
PAN contains nitrile group (-CN) which can be converted into carboxyl group (-COOH) or metal salt (-COOM) of carboxyl group under acid or alkaline condition, and is the main matrix for preparing carboxyl-containing material by chemical modification. There are two main methods of hydrolysis of PAN materials: acid-catalyzed hydrolysis and base-catalyzed hydrolysis. Wherein, the acid catalyzed hydrolysis usually takes a high-concentration inorganic acid solution as a reaction solution to hydrolyze the PAN fiber under the heating condition. A large amount of inorganic acid is used during the reaction, and high concentration of acid not only corrodes equipment but also makes post-treatment difficult. Hydrochloric acid is volatile, which makes it difficult to operate at boiling; high concentrations of sulfuric acid solutions may dissolve the PAN material, affecting the application of the hydrolysate.
Disclosure of Invention
In view of the above, the present invention provides a method for catalytically hydrolyzing Polyacrylonitrile (PAN) material under acidic conditions. According to the method, the catalyst is added into the reaction solution, so that the concentration of hydrogen ions in the reaction solution is reduced, and the hydrolysis rate of the PAN material in a low-concentration acidic solution is increased.
In order to achieve the purpose of the invention, the following technical scheme is provided.
A method for catalytically hydrolyzing polyacrylonitrile materials under acidic conditions, the method steps comprising:
adding a catalyst into the acidic solution to obtain a mixed solution, and heating to 60-130 ℃; and adding a PAN material into the mixed solution, reacting for 0.5-6 h, taking out the material after the reaction is finished, and washing to be neutral to obtain the PAN-COOH fiber.
The catalyst is bismuth nitrate oxidant or zinc chloride transition metal salt; preferably, the catalyst is bismuth nitrate, zinc chloride or nickel sulfate.
The acid solution is prepared from acid substances; preferably, the acidic substance is an inorganic acid; more preferably, the acidic material is sulfuric acid (H)2SO4) Hydrochloric acid (HCl) or nitric acid (HNO)3)。
Hydrogen ions (H) in the acidic solution+) The concentration of (B) is 1mol/L to 6 mol/L.
The solvent of the mixed solution is deionized water, ethanol, ethylene glycol, dimethylformamide or dimethyl sulfoxide; preferably, the solvent is deionized water.
The metal ions and H in the catalyst+The amount ratio of the substances (A) to (B) is 1:100 to 1: 10; preferably, the metal ions in the catalyst are reacted with H+The mass ratio of (a) to (b) is 1:50 to 1: 10.
The ratio of the volume (mL) of the mixed solution to the mass (g) of the PAN material is 100: 1-5: 1; preferably, the ratio of the volume of the mixed solution to the mass of the PAN fiber is 50: 1-8: 1.
The reaction temperature is preferably 80 ℃ to 120 ℃.
The PAN material comprises textile fibers, engineering fibers, yarns, gauze, non-woven fabrics, spunlaced fabrics and needled fabrics.
The mass transfer enhancement is preferably effected by stirring during the hydrolysis reaction.
Advantageous effects
1. The invention provides a method for catalytically hydrolyzing PAN material under acidic conditions, which hydrolyzes PAN material under low-concentration acidic solution by adding a catalyst. Compared with the prior art, the PAN material with unit mass is hydrolyzed by using the acidic solution with the same hydrogen ion concentration, the PAN-COOH fiber generated by the method has high carboxyl content and more sufficient reaction; in addition, the PAN material with the same amount is hydrolyzed to generate PAN-COOH fibers with the same amount, the method has the advantages of less usage amount of acidic substances, lower usage amount of hydrogen ions in the reaction process, lower production cost and more environment-friendly process conditions.
2. The method adopts the low-concentration acidic solution as the reaction liquid to hydrolyze the PAN material, reduces the corrosion to equipment and the dissolution to the PAN material, and obtains the PAN-COOH fiber with higher strength.
Drawings
Fig. 1 is a graph of the infrared absorption spectrum of PAN textile fibers.
FIG. 2 is a graph showing an infrared absorption spectrum of PAN-COOH fibers obtained in example 1.
Detailed Description
The invention is described in detail below with reference to the drawings and specific examples, but the invention is not limited thereto.
In the following examples:
(1) fourier transform infrared spectroscopy (FTIR): compacting a fiber sample by adopting an intelligent component of a Nicolet 6700 Fourier transform infrared spectrometer under the test condition of scanning wave number of 400-4000 cm-1Resolution of 4cm-1And the number of scans 32.
(2) The method for measuring the carboxyl content is an acid-base titration method, and specifically comprises the following steps:
1g of product to be detected is accurately weighed: shaking and reacting in 100mL of 0.1mol/L standard sodium hydroxide solution for 30min, taking 20mL of supernatant, titrating by using 0.1mol/L standard hydrochloric acid solution, and calculating the content of carboxyl.
(3) Testing the fiber strength:
using a Uster Hvi 1000 fiber tester: manufactured by the swiss Uster company; the breaking strength of the fibers to be tested was measured according to the method specified in GB/T14337-1993 test methods for breaking Strength and elongation of synthetic staple fibers.
(4) The length of the PAN textile fibers was 38 mm.
Comparative example 1
Heating 200ml of 3mol/L sulfuric acid solution to 100 ℃, wherein the solvent of the sulfuric acid solution is deionized water, adding 4g of PAN textile fiber, carrying out reflux reaction for 2 hours, stirring by a magnetic rotor, taking out the fiber after the reaction is finished, and washing the fiber to be neutral by the deionized water to obtain a final product.
The structure of the final product of this comparative example was determined by infrared spectroscopy at 2240cm-1The relative intensity of the characteristic peaks on the left and right is weakened, which shows that the relative content of-CN groups in the product is reduced, and the final product obtained by the comparative example is 3400cm-1The absorption peak of the right and left active hydrogen is strong and sharp, 1069.61cm-1The C-O stretching vibration absorption peak is widened and strengthened and is 1739.23cm-1The presence of the stretching vibration absorption peak of C ═ O indicates that the final product had a — COOH group, and it was found that the final product obtained in this comparative example was PAN-COOH fiber.
The carboxyl content of the PAN-COOH fiber prepared in the comparative example is 0.28mmol/g measured by an acid-base titration method; the fiber strength test shows that the breaking strength of the PAN-COOH fiber prepared by the comparative example is 3.21 cN/dtex.
Comparative example 2
Heating 200ml of 1mol/L nitric acid solution to 100 ℃, wherein the solvent of the nitric acid solution is deionized water, adding 4g of PAN textile fiber, carrying out reflux reaction for 2h, stirring by a magnetic rotor, taking out the fiber after the reaction is finished, and washing the fiber to be neutral by the deionized water to obtain a final product.
The structure of the final product of this comparative example was determined by infrared spectroscopy at 2240cm-1The relative intensity of the characteristic peaks on the left and right is weakened, which shows that the relative content of-CN groups in the product is reduced, and the final product obtained by the comparative example is 3400cm-1The absorption peak of the right and left active hydrogen is strong and sharp, 1069.61cm-1The C-O stretching vibration absorption peak is widened and strengthened and is 1739.23cm-1Has a stretching vibration absorption peak of C ═ O, which indicates that the final product has a-COOH group, wherebyIt can be seen that the final product obtained in this comparative example was PAN-COOH fiber.
The carboxyl content of the PAN-COOH fiber prepared in the comparative example is 0.11mmol/g measured by an acid-base titration method; the fiber strength test shows that the breaking strength of the PAN-COOH fiber prepared by the comparative example is 4.45 cN/dtex.
Example 1
Adding 8.00g of bismuth nitrate into 200ml of nitric acid solution with the concentration of 1mol/L, wherein the solvent of the nitric acid solution is deionized water, bismuth ions and H+The mass ratio of the materials is 1:10, the mixture is heated to 100 ℃, 4g of PAN textile fiber is added into the mixed aqueous solution, the mixture is refluxed and reacted for 2 hours, a magnetic rotor is used for stirring, after the reaction is finished, the fiber is taken out and washed to be neutral by deionized water, and a final product is obtained.
The structure of the final product of this example was examined by infrared spectroscopy, and the results are shown in FIG. 2; the characteristic peak of infrared absorption of the-CN group (2243.09 cm) can be seen from the infrared absorption spectrum of PAN textile fiber in FIG. 1-1) Strong and sharp, indicating a high content of-CN groups. In FIG. 2 the-CN group is at 2240cm-1The relative intensity of the left and right characteristic peaks is obviously weakened compared with that of figure 1, which shows that the relative content of-CN groups is reduced, 3400cm-1The absorption peak of the right and left active hydrogen is strong and sharp, 1069.61cm-1The C-O stretching vibration absorption peak is widened and strengthened and is 1739.23cm-1The presence of a stretching vibration absorption peak of C ═ O indicates that a large number of — COOH groups are present in the final product, and it is understood that the final product obtained in this example is PAN-COOH fiber.
The carboxyl content of the PAN-COOH fiber prepared in the example was determined to be 0.36mmol/g by acid-base titration. The fiber strength test shows that the breaking strength of the PAN-COOH fiber prepared in the embodiment is 4.27 cN/dtex.
Example 2
Adding 1.40g of zinc chloride into 200ml of hydrochloric acid solution with the concentration of 2mol/L, wherein the solvents of the hydrochloric acid solution are deionized water, zinc ions and H+The mass ratio of the materials is 1:20, the mixture is heated to 100 ℃, 4g of PAN textile fiber is added into the mixed solution, the mixture is refluxed and reacted for 2 hours, a magnetic rotor is used for stirring, after the reaction is finished, the fiber is taken out,washing with deionized water to neutrality to obtain the final product.
The structure of the final product of this example was determined by infrared spectroscopy at 2240cm-1The relative intensity of the characteristic peaks on the left and right is weakened, which indicates that the relative content of-CN groups in the product is reduced, and the final product obtained in the example is 3400cm-1The absorption peak of the right and left active hydrogen is strong and sharp, 1069.61cm-1The C-O stretching vibration absorption peak is widened and strengthened and is 1739.23cm-1The presence of a stretching vibration absorption peak of C ═ O indicates that a large number of — COOH groups are present in the final product, and it is understood that the final product obtained in this example is PAN-COOH fiber.
The carboxyl content of the PAN-COOH fiber prepared in the example was determined to be 0.40mmol/g by acid-base titration. The fiber strength test shows that the breaking strength of the PAN-COOH fiber prepared in the embodiment is 4.22 cN/dtex.
Example 3
Adding 2.20g of nickel sulfate into 200ml of sulfuric acid solution with the concentration of 1mol/L, wherein the solvent of the sulfuric acid solution is deionized water, zinc ions and H+The mass ratio of the materials is 1:50, the mixture is heated to 100 ℃, 4g of PAN textile fiber is added into the mixed solution, the mixture is refluxed and reacted for 2 hours, a magnetic rotor is used for stirring, after the reaction is finished, the fiber is taken out and washed to be neutral by deionized water, and a final product is obtained.
The structure of the final product of this example was determined by infrared spectroscopy at 2240cm-1The relative intensity of the characteristic peaks on the left and right is weakened, which indicates that the relative content of-CN groups in the product is reduced, and the final product obtained in the example is 3400cm-1The absorption peak of the right and left active hydrogen is strong and sharp, 1069.61cm-1The C-O stretching vibration absorption peak is widened and strengthened and is 1739.23cm-1The presence of a stretching vibration absorption peak of C ═ O indicates that a large number of — COOH groups are present in the final product, and it is understood that the final product obtained in this example is PAN-COOH fiber.
The carboxyl content of the PAN-COOH fiber prepared in the example was determined to be 0.39mmol/g by acid-base titration. The fiber strength test shows that the breaking strength of the PAN-COOH fiber prepared in the embodiment is 4.23 cN/dtex.
The carboxyl content and the breaking strength of the PAN-COOH fibres obtained in the respective proportions and examples were compared, the results being shown in table 1 (below):
TABLE 1 comparison of the carboxyl content of PAN-COOH fibers
As can be seen from Table 1, the PAN-COOH fibers prepared in examples 1 to 3 have the fiber carboxyl group content remarkably higher than that of comparative example 1, the fiber strength remarkably higher than that of comparative example 1, and the H content of the acid solution+The concentration is also lower; according to the data of the comparative example 2 and the example 1, the PAN-COOH fiber prepared by the method has high carboxyl content and more sufficient reaction when the PAN material with unit mass is hydrolyzed by the acidic solution with the same hydrogen ion concentration; in conclusion, compared with the prior art, the PAN-COOH fiber prepared by the method disclosed by the invention contains a large amount of carboxyl and has good strength.
The present invention includes, but is not limited to, the above embodiments, and any equivalent substitutions or partial modifications made under the principle of the spirit of the present invention should be considered as being within the scope of the present invention.
Claims (10)
1. A method for catalyzing and hydrolyzing polyacrylonitrile materials under acidic conditions is characterized in that: the method comprises the following steps:
adding a catalyst into the acidic solution to obtain a mixed solution, and heating to 60-130 ℃; adding a PAN material into the mixed solution, reacting for 0.5-6 h, taking out the material after the reaction is finished, and washing to be neutral to obtain PAN-COOH fibers;
the catalyst is bismuth nitrate oxidant or zinc chloride transition metal salt;
the acid solution is prepared from acid substances;
the concentration of hydrogen ions in the acid solution is 1-6 mol/L;
the solvent of the mixed solution is deionized water, ethanol, glycol, dimethylformamide or dimethyl sulfoxide;
the mass ratio of the metal ions to the hydrogen ions in the catalyst is 1:100 to 1: 10;
the ratio of the volume (mL) of the mixed solution to the mass (g) of the PAN material is 100: 1-5: 1.
2. The method of claim 1, wherein the polyacrylonitrile material is catalytically hydrolyzed under an acidic condition: the catalyst is bismuth nitrate, zinc chloride or nickel sulfate.
3. The method of claim 1, wherein the polyacrylonitrile material is catalytically hydrolyzed under an acidic condition: the acidic substance is an inorganic acid.
4. The method of claim 3, wherein the polyacrylonitrile material is catalyzed and hydrolyzed under an acidic condition: the acidic substance is sulfuric acid, hydrochloric acid or nitric acid.
5. The method of claim 1, wherein the polyacrylonitrile material is catalytically hydrolyzed under an acidic condition: the mass ratio of the metal ions to the hydrogen ions in the catalyst is 1: 50-1: 10.
6. The method of claim 1, wherein the polyacrylonitrile material is catalytically hydrolyzed under an acidic condition: the solvent of the mixed solution is deionized water.
7. The method of claim 1, wherein the polyacrylonitrile material is catalytically hydrolyzed under an acidic condition: the ratio of the volume (mL) of the mixed solution to the mass (g) of the PAN fiber is 50: 1-8: 1.
8. The method of claim 1, wherein the polyacrylonitrile material is catalytically hydrolyzed under an acidic condition: the reaction temperature is 80-120 ℃.
9. The method of claim 1, wherein the polyacrylonitrile material is catalytically hydrolyzed under an acidic condition: the method increases agitation during the reaction.
10. The method of claim 1, wherein the polyacrylonitrile material is catalytically hydrolyzed under an acidic condition:
the catalyst is bismuth nitrate, zinc chloride or nickel sulfate;
the acidic substance is sulfuric acid, hydrochloric acid or nitric acid;
the mass ratio of metal ions to hydrogen ions in the catalyst is 1: 50-1: 10;
the solvent of the mixed solution is deionized water;
the ratio of the volume (mL) of the mixed solution to the mass (g) of the PAN fiber is 50: 1-8: 1;
the reaction temperature is 80-120 ℃;
the method increases agitation during the reaction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011205465.2A CN112442892B (en) | 2020-11-02 | 2020-11-02 | Method for catalytically hydrolyzing polyacrylonitrile material under acidic condition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011205465.2A CN112442892B (en) | 2020-11-02 | 2020-11-02 | Method for catalytically hydrolyzing polyacrylonitrile material under acidic condition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112442892A true CN112442892A (en) | 2021-03-05 |
| CN112442892B CN112442892B (en) | 2023-02-28 |
Family
ID=74736626
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011205465.2A Active CN112442892B (en) | 2020-11-02 | 2020-11-02 | Method for catalytically hydrolyzing polyacrylonitrile material under acidic condition |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112442892B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113882153A (en) * | 2021-11-02 | 2022-01-04 | 中国船舶重工集团公司第七一八研究所 | Method for preparing carboxylic acid fiber by catalytic hydrolysis of polyacrylonitrile |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4820872A (en) * | 1984-07-17 | 1989-04-11 | Allied Colloids Ltd. | Process for hydrolyzing nitriles |
| US6509439B1 (en) * | 2000-04-14 | 2003-01-21 | E. I. Du Pont De Nemours And Company | Process for the production of polyamides from dinitriles and diamines |
| CN106928942A (en) * | 2017-03-10 | 2017-07-07 | 石家庄华莱鼎盛科技有限公司 | Fluid loss additive for boring fluid AM/AA/ hydrolyzed polyacrylonitrile ammonium salt copolymer aquas and preparation method thereof |
| CN107146915A (en) * | 2017-04-10 | 2017-09-08 | 中山大学 | A kind of preparation method of porous bismuth carbon composite |
| CN111100022A (en) * | 2019-10-30 | 2020-05-05 | 石家庄市栾城区华英工贸有限责任公司 | Method for preparing carboxylic acid compounds by catalyzing nitrile compounds to hydrolyze with Lewis acid |
-
2020
- 2020-11-02 CN CN202011205465.2A patent/CN112442892B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4820872A (en) * | 1984-07-17 | 1989-04-11 | Allied Colloids Ltd. | Process for hydrolyzing nitriles |
| US6509439B1 (en) * | 2000-04-14 | 2003-01-21 | E. I. Du Pont De Nemours And Company | Process for the production of polyamides from dinitriles and diamines |
| CN106928942A (en) * | 2017-03-10 | 2017-07-07 | 石家庄华莱鼎盛科技有限公司 | Fluid loss additive for boring fluid AM/AA/ hydrolyzed polyacrylonitrile ammonium salt copolymer aquas and preparation method thereof |
| CN107146915A (en) * | 2017-04-10 | 2017-09-08 | 中山大学 | A kind of preparation method of porous bismuth carbon composite |
| CN111100022A (en) * | 2019-10-30 | 2020-05-05 | 石家庄市栾城区华英工贸有限责任公司 | Method for preparing carboxylic acid compounds by catalyzing nitrile compounds to hydrolyze with Lewis acid |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113882153A (en) * | 2021-11-02 | 2022-01-04 | 中国船舶重工集团公司第七一八研究所 | Method for preparing carboxylic acid fiber by catalytic hydrolysis of polyacrylonitrile |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112442892B (en) | 2023-02-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109322160B (en) | Cross-linked PAN-COOH fiber and preparation method thereof | |
| CN112442892B (en) | Method for catalytically hydrolyzing polyacrylonitrile material under acidic condition | |
| Li et al. | Preparation and catalytic performance of Fe (III)-citric acid-modified cotton fiber complex as a novel cellulose fiber-supported heterogeneous photo-Fenton catalyst | |
| CN1811021A (en) | Functional fiber and the multifunctional fiber thereof | |
| CN110124390B (en) | Preparation method of denitration filter material | |
| CN105484012B (en) | A kind of polyacrylonitrile carbon fiber surface treatment method and device | |
| CN106622166A (en) | Polyaspartic acid and bentonite composite material for removing heavy metal ions and preparation method thereof | |
| CN109985668B (en) | Chitosan hybridized bismuth oxybromide micro-nano multi-layer material and preparation and application thereof | |
| CN106362804A (en) | Magnetic carbon-based solid acid catalyst as well as preparation method and application thereof | |
| CN112281471A (en) | Method for catalytically hydrolyzing polyacrylonitrile material under alkaline condition | |
| CN101125294B (en) | Modified active carbon catalyst and its preparation method and application | |
| CN108212187A (en) | Fe adulterates Bi2O2CO3Preparation method and Fe the doping Bi of photochemical catalyst2O2CO3Photochemical catalyst | |
| CN104817643B (en) | Bacteria cellulose homogeneously prepares the preparation method of cationic flocculant | |
| CN116814084A (en) | Sustained-release sodium sarcosinate and preparation method thereof | |
| CN113882153B (en) | Method for preparing carboxylic acid fiber by polyacrylonitrile catalytic hydrolysis | |
| CN1508078A (en) | Method for preparing modified hyphostroma water treatment chemical | |
| CN112850860B (en) | Preparation method and application of nitrogen-doped ordered mesoporous carbon electrode | |
| CN101260187B (en) | Method for preparing nano-stage naphthylamine sulfonate and aniline copolymer | |
| CN111508731B (en) | Polyaniline composite conductive film based on egg inner membrane and preparation method and application thereof | |
| CN114308133A (en) | Fe-loaded iron core3O4Nano particle composite fiber membrane as heterogeneous Fenton catalyst and preparation method thereof | |
| CN116943733A (en) | Preparation method and application of PVA-co-PE nanofiber membrane supported cobalt catalyst | |
| CN109317214A (en) | A kind of load of transition metal together with ammonia deuteration self assembly polyacrylonitrile microballoon catalyst and the preparation method and application thereof | |
| CN115404696B (en) | Dopamine quinone fiber and preparation method, application and application method thereof | |
| He et al. | Preparation, Surface Acidity and Catalytic Esterification Activity of Solid Acid S2O2-8/TiO2-La2O3 | |
| CN111548442B (en) | Surface hydrophilic treatment agent, preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |