CN1126636A - Acid-gas adsorbing fibre and its prodn technology and equipment - Google Patents
Acid-gas adsorbing fibre and its prodn technology and equipment Download PDFInfo
- Publication number
- CN1126636A CN1126636A CN 95116025 CN95116025A CN1126636A CN 1126636 A CN1126636 A CN 1126636A CN 95116025 CN95116025 CN 95116025 CN 95116025 A CN95116025 A CN 95116025A CN 1126636 A CN1126636 A CN 1126636A
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- Prior art keywords
- acid
- fibre
- gas adsorbing
- polyethylene polyamine
- acrylic fiber
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Abstract
The said adsorbing fibre is produced with commercial acrylic fibre and polyvinyl polyamine as raw material. The lowest weight ratio of acrylic fibre to polyvinyl polyamine is 1 to 2, and they react in a reactor with stirring wavewheel and spinning tank in the reaction temp of 100-160 deg.C. The product has low degree of cross linking and great adsorption capacity, the static adsorption capacity for HCl solution can reach 10.02 mmol each gram of fibre, and the dynamic adsorption capacity for SO2 can reach 190 mg each gram of fibre.
Description
The present invention relates to a kind of fine chemical product, relate in particular to a kind of acid waste gas, aerosol (as: SO that contains multiple organic amine functional group, is used for the various industry of adsorption filtration and lives and produced
2, HCL, HF, NO
xAnd human body pin odour etc.) acid-gas adsorbing fibre and preparation technology and device.
At present, the existing multiple functional fibre material that can be used for adsorption filtration deleterious acidic gas comes out, and successfully these new materials is used for the protective face mask of labour protection, in the pernicious gas adsorptive purifier.European patent EP 194766 has been reported and has been utilized acrylic fiber and 4.8% hydrazine solution 127 ℃ of reactions down, and after the drying processing, the method that contains the ion-exchange fibre of imidazoline group again with reacting ethylenediamine preparation in 3 hours, U, S, S, R SU1512984, JP62298359 and former Soviet Union's document " the VION anion-exchange fibre is to the equilibrium adsorption research of sour gas; " " chemical fibre " magazine 62 (6), 1315 (1989) " and document " Thesynthesis, structure and properties of New fibrousIon Exchangers "; " Reactive Polymers "; 7 (1988); 159 have reported and utilize acrylic fiber successively and aqueous hydroxylamine solution and ethylenediamine; the polyethylene polyamine solution reaction, and utilize and the functional fibre material that the method preparation can be adsorbed different pernicious gases such as react behind the poly-sour fiber radiation grafting.But these preparation technologies are more loaded down with trivial details, and the adsorption capacity of gained functional fibre material is lower, and dynamic adsorption also remains further to be improved.
The purpose of this invention is to provide that a kind of production technology is simple, the reaction time is short, production equipment is simple, good product quality, to the acid-gas adsorbing fibre that adsorption capacity is big, dynamic adsorption is good and the preparation technology and the device of sour gas.
Technical scheme of the present invention is achieved in that
A kind of acid-gas adsorbing fibre, it adopts general goods acrylic fiber, polyethylene polyamine is raw material, wherein the polyethylene polyamine chemical formula is NH
2(CH
2CH
2NH)
nCH
2-CH
2NH
2, n=0 in the formula-5, acrylic fiber: polyethylene polyamine (weight ratio) is minimum to be controlled to be 1: 2.
The line density of acrylic fiber is 1.5-10.0D, and length is 30-120mm
Polyethylene polyamine can be triethylene tetramine, diethylenetriamine, ethylenediamine.
Polyethylene polyamine can be triethylene tetramine, diethylenetriamine, the ethylenediamine of any weight ratio.
The preparation technology who prepares above-mentioned acid-gas adsorbing fibre is: reinforced-temperature reaction-as to dry-wash-as to dry, and be raw material wherein with general goods acrylic fiber, polyethylene polyamine, acrylic fiber: polyethylene polyamine (weight ratio) is minimum to be controlled at 1: 2; Reaction temperature is controlled at 100-160 ℃.
Polyethylene polyamine is triethylene tetramine, diethylenetriamine, ethylenediamine.
Polyethylene polyamine can be triethylene tetramine, the diethylenetriamine of any weight ratio, ethylenediamine.
Reaction temperature preferably is controlled at 120-150 ℃.
The device of preparation acid-gas adsorbing fibre is the reactor of a band heating jacket, reactor has loam cake (2), condenser (1), oil bath device (3), by electric heater (4) is arranged in the bath apparatus (3), be a centrifuge dripping bucket (5) in the middle of the reactor wherein, centrifuge dripping bucket (5) is contained on the shaft of stirring motor (6), one impeller also is housed on the stirring motor axle in centrifuge dripping bucket (5) stirs (7), centrifuge dripping bucket (5) and impeller stirring (7) are by a clutch separation or be fixed in substep or synchronous rotation the on the motor shaft.
Good effect of the present invention is:
1, the degree of cross linking of this acid-gas adsorbing fibre is lower, thereby soft, and adsorption capacity increases, and can reach 10.02mmol (HCL)/g (fiber) to the static adsorption capacity of HCL solution, and dynamic adsorption can reach 190mg (SO
2)/g (fiber).
2, preparation technology is simple, owing to do not use reaction dissolvent, so raw material directly contacts, the reaction time is short, saves the separated from solvent step simultaneously.
3, production technology adopts the special reactor that has impeller stirring, centrifuge dripping bucket, make the production of adsorbing fiber in an equipment, to finish, wherein impeller stirs and makes fiber liquid-solid two-phase in course of reaction fully contact, the hot-spot phenomenon reduces, and the fibre machinery performance did not suffer havoc.Simultaneously, the employing that dries device in the reactor makes reaction finish acid adsorbing fiber under the condition of high temperature of back to separate with polyethylene polyamine fast and finish operations such as washing, drying continuously.
Below in conjunction with embodiment the present invention is described in further detail:
Embodiment 1, with technical grade polyethylene polyamine 64Kg, acrylic fiber 8Kg (1.5D, 65mm) add in the reaction unit, in 45 minutes, reaction temperature is risen to 135 ℃, and kept 80 minutes, during entire reaction, start impeller and stir the good stirring that keeps fiber and reactant liquor, after reaction finishes, residual reaction liquid is emitted, the centrifugal reactant liquor that is attached on the fiber of removing after distilled water washing 4-5 times, dries naturally, get adsorbing fiber 17Kg, fiber is 8.44mmol/g to the static adsorption capacity of hydrochloric acid solution.
Embodiment 2, with technical grade triethylene tetramine 300g, acrylic fiber 150g (3D, 65mm) add in the reaction unit, in 60 minutes, reaction temperature is risen to 100 ℃, be incubated 60 minutes, during entire reaction, start impeller and stir and to stir material, reaction finishes the centrifugal reactant liquor that is attached on the fiber of removing in back, dries naturally with behind the distilled water washing the fibre 5 times, get adsorbing fiber 300g, fiber is 7.86mmol/g to the static adsorption capacity of hydrochloric acid solution.
Embodiment 3, technical grade diethylenetriamine 60Kg is added in the reaction unit, in 60 minutes, reaction temperature is risen to 150 ℃, (6D 120mm) adds in the reaction unit, keeps 30 minutes at 160 ℃ with acrylic fiber 10Kg, after emitting reactant liquor, the centrifugal reactant liquor that is attached on the fiber of removing behind distilled water washing the fibre 4-5 times, dries naturally, get adsorbing fiber 22Kg, fiber is 10.02mmol/g to the static adsorption capacity of hydrochloric acid solution.
Embodiment 4, technical grade diethylenetriamine 100Kg is added in the reaction unit, in 60 minutes, reaction temperature is risen to 150 ℃, (10D 90mm) adds in the reaction unit, keeps 30 minutes at 160 ℃ with acrylic fiber 10Kg, after emitting reactant liquor, the centrifugal reactant liquor that is attached on the fiber of removing behind distilled water washing the fibre 4-5 times, dries naturally, get adsorbing fiber 22Kg, fiber is 10.02mmol/g to the static adsorption capacity of hydrochloric acid solution.
Embodiment 5, with SILVER REAGENT ethylenediamine 500g, industry acrylic fiber 100g (2D, 65mm) add in the reaction unit, be heated to 105 ℃, after the insulation reaction 60 minutes, take out fiber, with distilled water, hydrochloric acid, sodium carbonate liquor washing, be washed till neutrality with distilled water at last, vacuum drying respectively, get adsorbing fiber 120g, adsorbing fiber is 2.78mmol/g to the static adsorption capacity of hydrochloric acid solution.
Embodiment 6, with the different n value polyethylene polyamine mixture 64Kg that used once, acrylic fiber 8Kg adds in the reaction unit, after evenly being warming up to 120 ℃, kept this temperature 80 minutes, in whole intensification, stir stirring by impeller between soak and keep good dynamic contact between reaction system each several part temperature uniformity and the raw material, after reaction finishes, by the bottom baiting valve residual reaction liquid is emitted, the centrifugal device of opening in the reaction unit is removed the reactant liquor that is attached on the fiber, (the polyethylene polyamine reaction liquid that these two parts reclaim can be stored the adsorbing fiber preparation that is used for next time), with distilled water cleaning product 4 times to washings pH≤7.5, naturally dry to fiber moisture≤15%, get product adsorbing fiber 17Kg, adsorbing fiber is 8.03mmol/g to the static adsorption capacity of hydrochloric acid.
The assay method of the static adsorption capacity of acid-gas adsorbing fibre is as follows: earlier ion-exchange fibre is handled through the 0.5mol/L sodium hydroxide solution, the distilled water washing, vacuum drying is to constant weight, accurately take by weighing 0.1g, put in the 50ml conical flask and to add 25ml hydrochloric acid and sodium chloride concentration and be respectively 0.1 and the 1.0mol/L mixed liquor, vibration and remove the bubble that is attached on the fiber after, sealing was placed 48 hours.Use the standard caustic soda solution titration, be calculated as follows out saturated adsorption capacity Qw (unit: the mmol/g fiber) be:
In the formula: Q
W---the adsorption capacity (mmol/g) of fiber
C---standard caustic soda solution concentration (mol/L)
V
0---fixed clearly blank used sodium hydroxide solution body (ml)
V
1---quality of fiber (g)
Dynamic adsorption capacity is pressed GB2892.7-8 standard testing
This acid-gas adsorbing fibre is to SO2, the Dynamic Adsorption of the Dynamic Adsorption of HCL and Static Adsorption performance and other products and the contrast of Static Adsorption The performance test results be such as following table:
| Name of product | Static Adsorption capacity mmol (HCL)/g | Attitude adsorption capacity mg (SO2)/g |
| This product | 7—10 | 190 |
| No. 7 acid-proof granular activated carbons | 2.5 | 18 |
| Former Soviet Union VION fiber | 2.1 | |
| Former Soviet Union FibanAK-22 | 4.5—7 | 135 |
Claims (10)
1, a kind of acid-gas adsorbing fibre is characterized in that it adopts general goods acrylic fiber, polyethylene polyamine is raw material, and the polyethylene polyamine chemical formula is NH
2(CH
2CH
2NH)
nCH
2-CH
2NH
2, n=0-5, acrylic fiber: polyethylene polyamine (weight ratio) is minimum to be controlled to be 1: 2.
2, acid-gas adsorbing fibre according to claim 1 is characterized in that the line density of acrylic fiber is 1.5-10.0D, and length is 40-120mm
3, acid-gas adsorbing fibre according to claim 2 is characterized in that polyethylene polyamine can be triethylene tetramine, diethylenetriamine, ethylenediamine.
4, acid-gas adsorbing fibre according to claim 1 is characterized in that polyethylene polyamine can be triethylene tetramine, diethylenetriamine, the ethylenediamine of arbitrary proportion.
5, the preparation technology of acid-gas adsorbing fibre according to claim 1 comprises: reinforced-temperature reaction-as to dry-wash-as to dry, it is characterized in that with general goods acrylic fiber, polyethylene polyamine be raw material, the raw material ratio acrylic fiber: polyethylene polyamine (weight ratio) is minimum for being controlled to be 1: 2, and the polyethylene polyamine chemical formula is NH
2(CH
2CH
2NH)
nCH
2-CH
2NH
2, n=0-5, reaction temperature is controlled at 100-160 ℃.
6, the preparation technology of acid-gas adsorbing fibre according to claim 5, the line density that it is characterized in that acrylic fiber is 1.5-10.0D, length is 40-120mm.
7, the preparation technology of acid-gas adsorbing fibre according to claim 6 is characterized in that polyethylene polyamine can be triethylene tetramine, diethylenetriamine, ethylenediamine.
8, acid-gas adsorbing fibre according to claim 6 is characterized in that polyethylene polyamine can be triethylene tetramine, diethylenetriamine, the ethylenediamine of arbitrary proportion.
9, the preparation technology of acid-gas adsorbing fibre according to claim 5 is characterized in that reaction temperature is controlled at 120-150 ℃.
10, the process units according to the described acid-gas adsorbing fibre of claim 1-9 is the reactor of a band heating jacket, reactor has condenser (1), oil bath heater (3), electric heater unit (4) and stirring, it is characterized in that in the middle of the reactor be a centrifuge dripping bucket (5), centrifuge dripping bucket (5) activity is contained on the shaft of stirring motor (6), stirring in centrifuge dripping bucket (5) trembled impeller stirring (7) also is housed on the motor shaft, and centrifuge dripping bucket (5) stirs (7) with impeller and rotates step by step by motor shaft.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95116025A CN1046431C (en) | 1995-10-07 | 1995-10-07 | Acid gas adsorption fiber and preparation process and device thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95116025A CN1046431C (en) | 1995-10-07 | 1995-10-07 | Acid gas adsorption fiber and preparation process and device thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1126636A true CN1126636A (en) | 1996-07-17 |
| CN1046431C CN1046431C (en) | 1999-11-17 |
Family
ID=5080734
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN95116025A Expired - Fee Related CN1046431C (en) | 1995-10-07 | 1995-10-07 | Acid gas adsorption fiber and preparation process and device thereof |
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| Country | Link |
|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103663621A (en) * | 2013-11-13 | 2014-03-26 | 郑州大学 | Method for treating hexavalent chromium wastewater with weak base ion exchange fiber |
| CN105498672A (en) * | 2016-01-14 | 2016-04-20 | 河北工业大学 | Production device and preparation method of composite phase-change particles |
| CN105672004A (en) * | 2016-04-18 | 2016-06-15 | 河南工程学院 | Fluorescein dyeing and multifunctional finishing method for acrylic fabric |
| CN111282380A (en) * | 2020-03-26 | 2020-06-16 | 河南中白环境科学技术研究院有限公司 | Treatment process and treatment device for high-concentration hydrogen sulfide gas |
| CN114042437A (en) * | 2021-11-12 | 2022-02-15 | 河南省科学院化学研究所有限公司 | Preparation process of amino weakly-alkaline anion exchange fiber |
| CN116178211A (en) * | 2022-12-10 | 2023-05-30 | 昊华气体有限公司 | Method for removing high-content acidic impurities in perfluoroisobutyronitrile crude gas |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1081176A1 (en) * | 1979-10-16 | 1984-03-23 | Кемеровский Научно-Исследовательский Институт Химической Промышленности Кемеровского Научно-Производственного Объединения "Карболит" | Process for preparing anionite |
| SU1087573A1 (en) * | 1983-02-04 | 1984-04-23 | Ленинградский ордена Трудового Красного Знамени институт текстильной и легкой промышленности им.С.М.Кирова | Method of producing ion-exchange polyacryl-nitryl fibre |
| US4806019A (en) * | 1985-09-03 | 1989-02-21 | Nova Scotia Research Foundation Corporation | Method and apparatus for mixing two or more components such as immiscible liquids |
-
1995
- 1995-10-07 CN CN95116025A patent/CN1046431C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103663621A (en) * | 2013-11-13 | 2014-03-26 | 郑州大学 | Method for treating hexavalent chromium wastewater with weak base ion exchange fiber |
| CN103663621B (en) * | 2013-11-13 | 2015-11-04 | 郑州大学 | Utilize the method for weak base ion-exchange fiber process hexavalent chromium wastewater |
| CN105498672A (en) * | 2016-01-14 | 2016-04-20 | 河北工业大学 | Production device and preparation method of composite phase-change particles |
| CN105498672B (en) * | 2016-01-14 | 2017-04-26 | 河北工业大学 | Production device and preparation method of composite phase-change particles |
| CN105672004A (en) * | 2016-04-18 | 2016-06-15 | 河南工程学院 | Fluorescein dyeing and multifunctional finishing method for acrylic fabric |
| CN111282380A (en) * | 2020-03-26 | 2020-06-16 | 河南中白环境科学技术研究院有限公司 | Treatment process and treatment device for high-concentration hydrogen sulfide gas |
| CN114042437A (en) * | 2021-11-12 | 2022-02-15 | 河南省科学院化学研究所有限公司 | Preparation process of amino weakly-alkaline anion exchange fiber |
| CN114042437B (en) * | 2021-11-12 | 2023-11-10 | 河南省科学院化学研究所有限公司 | Preparation process of amino weak-alkaline anion exchange fiber |
| CN116178211A (en) * | 2022-12-10 | 2023-05-30 | 昊华气体有限公司 | Method for removing high-content acidic impurities in perfluoroisobutyronitrile crude gas |
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| Publication number | Publication date |
|---|---|
| CN1046431C (en) | 1999-11-17 |
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