CN1035428C - Circular ammonia no-hydrogen deoxygen purify system for drying polyamide fibre section - Google Patents

Circular ammonia no-hydrogen deoxygen purify system for drying polyamide fibre section Download PDF

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Publication number
CN1035428C
CN1035428C CN94107023A CN94107023A CN1035428C CN 1035428 C CN1035428 C CN 1035428C CN 94107023 A CN94107023 A CN 94107023A CN 94107023 A CN94107023 A CN 94107023A CN 1035428 C CN1035428 C CN 1035428C
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China
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nitrogen
hydrogen
oxygen
drying
nitrogen gas
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CN94107023A
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CN1099718A (en
Inventor
郑质文
黄哲
苏化东
孟崇志
韩存田
田璠
杨增堂
王丽雅
杨振兴
刘丰丰
芦银全
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SHANXI PROV CHEMICAL FIBRE INST
Shanxi Institute of Coal Chemistry of CAS
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SHANXI PROV CHEMICAL FIBRE INST
Shanxi Institute of Coal Chemistry of CAS
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Abstract

The present invention provides a circular nitrogen gas no-hydrogen deoxidizing purification system for drying chinlon sections. For dehumidification and deoxidization, the present invention adopts the following method that (a), nitrogen gas containing oxygen and water is frozen to remove most of the water, and then, an adsorption agent is used for further adsorption and drying, so that the water content in the nitrogen gas is less than 38 ppm; (b), the dried nitrogen gas needs no hydrogen under the pressure of 0.01 to 0.8MPa and at a temperature of a normal temperature to 400 DEG C, and deoxidizers are directly used for deoxidization, so that the oxygen content in the nitrogen gas is less than 5 ppm. Since hydrogen is not required to be added to the nitrogen gas, the no-hydrogen purification system can omit devices for automatically and accurately tracking and detecting hydrogen and oxygen and accurately detecting and regulating gas flow. The present invention can simplify operation and maintenance, save a large amount of investment and eliminate unsafe hidden dangers.

Description

A kind of nitrogen deoxidizing purification method
The invention belongs to gas cleaning, particularly a kind of polyamide fibre section exsiccant nitrogen purge system.
The polyamide fibre section drying is an indispensable critical process during extrusion spinning is produced.The dry inert gas (being generally nitrogen) that its drying process normally will be heated to certain temperature feeds in the drying tower and directly contacts with moisture polyamide fibre section, and the heating section is also taken away wherein moisture, thereby reaches the purpose of chip drying.Exsiccant nitrogen has carried moisture and has discharged outside the tower in tower, must be with moisture removal before cyclically utilizing.In addition, moisture polyamide fibre section when advancing tower and nitrogen in working cycle, all can have a small amount of oxygen to enter system from the external world, these oxygen also must be removed before entering drying tower high temperature drying district.Therefore, be used for the purification of polyamide fibre section exsiccant circulating nitrogen gas, i.e. deoxidation, dehumidifying just become crucial link in the drying process.The used purification techniques of domestic imported unit is to allocate appropriate amount of hydrogen into as reductor in circulated inert gas, itself and oxygen is reacted and generation water, reaches the purpose of deoxidation, and then with cooling and sorbent material water is removed.The polyamide fibre section successive drying system that polyamide fibre factory and Changsha polyamide fibre factory are newly understood in Guangdong is an example.This method of joining the hydrogen deoxygenation must strict control be joined the hydrogen amount, residual oxygen is removed to the prerequisite of 5ppm level guaranteeing, and residual hydrogen should be low as far as possible.Therefore, in system, just need the high hydrogen of tolerance range, oxygen to detect and gas flow precision measurement, regulation device (domestic difficulty is still accomplished at present) from motion tracking.Like this, must influence the production domesticization of purification system, cause equipment manufacturing cost high.In addition,, therefore, all need to treat, have hidden danger by the Class A hazardous substance in storing, when using because hydrogen is flammable explosive gas.
The object of the present invention is to provide a kind of nitrogen no-hydrogen deoxygen purifying method, design is used for polyamide fibre section exsiccant circulating nitrogen gas no-hydrogen deoxygen purify system therefrom, have simple and convenient operation and maintenance, low, the safe and reliable characteristics of equipment cost, the suite of equipment manufacturing of can basing on our country.
The present invention is used for polyamide fibre section exsiccant circulating nitrogen gas no-hydrogen deoxygen purify system, adopts the deoxidation that dehumidifies of following method:
(a) it is freezing to contain the moisture nitrogen of oxygen, removes most of moisture, with the further adsorption dry of sorbent material, makes the water-content<38ppm in the nitrogen then,
(b) dried nitrogen is at 0.01~0.8MPa, need not join hydrogen under the condition of normal temperature~400 ℃, directly carries out deoxidation with reductor, makes the oxygen level<5ppm in the nitrogen.
The said nitrogen part that needs to purify of the present invention is the wet oxygen nitrogen that contains that contains of discharging from drying tower top in the system, and a part is to replenish the nitrogen of the system that enters.The latter can be the empty nitrogen that divides, and also can be the nitrogen of molecular sieve transformation absorption preparation, its oxygen level<0.1%.The used sorbent material in described freezing back can be silica gel, molecular sieve, aluminum oxide etc.The dried oxygen nitrogen that contains does not need to join hydrogen and directly carries out deoxidation with reductor, described reductor can be beyond the dehydrogenation other can with the material of oxygen generation chemical reaction, as metal or its suboxide, carbon or the like.The preferred carbon of the present invention is made 3093 serial catalyzing deoxidation agents of carrier, and this reductor deoxidation effect is good, easy to use, inexpensive, can directly buy from the market.This reductor utilizes the reducing property of carbon support itself oxygen removal in the nitrogen can be arrived<5ppm, makes oxygen be converted into carbonic acid gas, and the latter can not produce harmful effect in the polyamide fibre section drying process.Described system pressure is 0.01~0.3MPa preferably, preferably 260~360 ℃ of deoxidation temperature.
Accompanying drawing is depicted as the circulating nitrogen gas no-hydrogen deoxygen purify system general flow chart that designs according to aforesaid method.Among the figure: 1 polyamide fibre section drying, 2 dedustings, 3 superchargings, 4 coolings, 5 is freezing, 6 dryings, 7 secondary boosters, 8 heating (1), 9 deoxidations, 10 terminal dedustings, 11 under meters (1), 12 heating (2), 13 heating (3), 14 under meters (2).
As shown in the figure, cleaning system is connected with drying tower 1, contains oxygen and contains wet qualified circulating nitrogen gas for drying tower provides. Drying tower ejects the moisture oxygen nitrogen that contains that comes and returns drying tower 1 at dedusting 2, two closed circuits of supercharging 3 rear branches from the middle part of tower (partial circulating) and bottom (systemic circulation). Two closed circuit gases enter the technological requirement that drying tower is depended in tower position, tolerance, temperature and pressure. The nitrogen of partial circulating only needs temperature adjustment 13, metering 14, need not purify before entering tower, and its effect is to make into the wet section of tower to give heat to the required temperature of drying and remove portion of water. Systemic circulation nitrogen then must pass through removal moisture drying, deoxygenation, dedusting. Its program is: gas to be clean and additional nitrogen after aforementioned dedusting 1, the supercharging 2 converge, and cooling is 4 to room temperature, through freezing 5, remove contained most of water, enter drier 6 and remove residual moisture. Thereafter supercharging 7. Heating 8 enters degasifier 9, in the presence of catalyzing deoxidation agent, contained oxygen is taken off to<5ppm. Bring system into for preventing dust, further dedusting 10 of nitrogen after the dry deoxidation, through measuring 11, entering drying tower 1 after the temperature adjustment 12 from the bottom, directly contact with the section of motion from top to bottom at Ta Nei, reverse flow is discharged from cat head carrying the moisture content and a small amount of oxygen that remove behind the chip drying, afterwards enters respectively large and small closed circuit through dedusting 2, supercharging 3 again, so repeatedly, namely consist of circulating nitrogen gas no-hydrogen deoxygen purify system of the present invention. Oxygen in Nitrogen content<5ppm after the present invention purifies, one 50 ℃ of dew points, dust content 1 μ level<3/liter.
The nitrogen that the present invention is used for the slices of caprone drying does not have the hydrogen purification system, and the agent of employing no-hydrogen deoxygen removes the oxygen in the nitrogen. Owing to need not allocate hydrogen in the nitrogen, so can save pinpoint accuracy hydrogen, oxygen detects and gas flow accurate measurement, regulation device from motion tracking, not only make operation and safeguard simplification, and a complete set of equipment production of can basing on our country, thereby reduce investment outlay in a large number, also eliminated hidden danger.
The present invention not only can be used for nitrogen purge, also can be used for the deoxidizing purification of other inert gas.
Embodiment 1
The polyamide fibre section drying tower that drying tower adopts Chinese patent 90218528.4 to provide is equipped with the automatic adding of section system, and this tower top is the nitrogen relief outlet, in, a nitrogen inlet is respectively arranged at the bottom.In the purification system, adopt Stainless Steel Wire web filter and fiber cell filter respectively as coarse filtration and terminal fly-ash separator.The supercharging volute pump.Water cooler is a hot tube heat exchanger, further the cooling refrigerator.Dress proper silica gel and molecular sieve in the moisture eliminator.It is 3093 catalyzing deoxidation agents (this reductor once obtained national invention second prize in 1984, can buy from Shanxi Inst. of Coal Chemistry, Chinese Academy of Sciences) of carrier that reductor adopts with carbon.Gas is used the well heater temperature adjustment before going into tower.
Main operating parameters: from the nitrogen that drying tower comes out, flow 1100~1200mm 3/ hr, 60~85 ℃ of temperature, pressure 0.001~0.0015MPa, and have 30~60g/m 3Moisture, section dust and<oxygen of 50ppm.Partial circulating tolerance 700~800mm 3/ hr without purifying treatment, enters the middle part of drying tower behind heating temperature adjustment to 100~110 ℃; Go into pressure tower 0.01~0.02MPa, dew point-50 ℃, oxygen level<50ppm, dust content 0.001%.Systemic circulation tolerance 200~400mm 3/ hr, oxygen level 500~1000ppm, through water cooler, refrigerator be chilled to 3~8 ℃ remove water of condensation after, in moisture eliminator, remove residual moisture, through the booster fan supercharging, heating, go into deoxidation reactor, under 350 ℃, remove oxygen wherein, remove micronic dust with the terminal fly-ash separator again, after metering, heating temperature adjustment, enter the bottom of drying tower; Go into tower nitrogen pressure 0.02MPa, 105~120 ℃ of temperature, dew point<-50 ℃, oxygen level<5ppm, dust content 1 μ level<3/liter reach the index of introducing equipment fully, satisfy industrial requirement.
Embodiment 2
The suboxide that adopts manganese is as reductor (reductor code name: 401, can buy from Dalian Inst of Chemicophysics, Chinese Academy of Sciences).All the other are with embodiment 1.

Claims (5)

1. one kind is used for polyamide fibre section exsiccant nitrogen deoxidizing purification method, it is characterized in that adopting the deoxygenation that dehumidifies of following method:
(a). contain the moisture nitrogen of oxygen and dehumidify the sorbent material depth drying with cold method;
(b). dried nitrogen is at 0.01~0.8MPa, uses the reductor deoxidation under the condition of normal temperature-400 ℃.
The purification process that adopts aforesaid method and design has two loops: the tolerance of partial circulating is the 60-80% that drying tower is discharged tolerance, and this part contains and wetly contains oxygen nitrogen advance drying tower without purifying treatment after dedusting, supercharging, temperature adjustment, metering; The tolerance of systemic circulation is the 20-40% of drying tower output, and this part contains wet oxygen nitrogen and the system of containing and replenishes nitrogen through cooling, freezing, dry, supercharging, deoxidation, enters in the drying tower after dedusting, metering, temperature adjustment again.
2. the method for claim 1 is characterized in that described system pressure is 0.01-0.03MPa.
3. the method for claim 1 is characterized in that described reductor temperature is 260-360 ℃.
4. the method for claim 1 is characterized in that described reductor can be other reductor beyond the dehydrogenation.
5. the method for claim 1 is characterized in that described reductor can be 3093 serial reductors of carbon support.
CN94107023A 1994-06-08 1994-06-08 Circular ammonia no-hydrogen deoxygen purify system for drying polyamide fibre section Expired - Fee Related CN1035428C (en)

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CN94107023A CN1035428C (en) 1994-06-08 1994-06-08 Circular ammonia no-hydrogen deoxygen purify system for drying polyamide fibre section

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Application Number Priority Date Filing Date Title
CN94107023A CN1035428C (en) 1994-06-08 1994-06-08 Circular ammonia no-hydrogen deoxygen purify system for drying polyamide fibre section

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CN1035428C true CN1035428C (en) 1997-07-16

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Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106731785A (en) * 2016-11-16 2017-05-31 上海二十冶建设有限公司 It is a kind of to extend using the method for PPS filtrate bag-type duster filtering bag service lifes
CN106582235A (en) * 2016-11-30 2017-04-26 新疆兵团现代绿色氯碱化工工程研究中心(有限公司) Method for removing oxygen in chlorination reaction gas
CN109224846B (en) * 2018-10-23 2021-09-07 北京北氧特气工程技术有限公司 High-purity nitrogen gas purification device
CN110528092B (en) * 2019-09-06 2021-09-28 浙江大地蓝化纤有限公司 One-step production process of superfine nylon and polyester combined filament yarn
CN110817812A (en) * 2019-11-28 2020-02-21 潍坊伟士昕气体设备有限公司 Small-size high-purity nitrogen generator
CN113244766A (en) * 2020-02-10 2021-08-13 新特能源股份有限公司 Single crystal furnace tail gas purification and recovery system and method

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN85102704A (en) * 1985-04-01 1986-09-24 中国科学院大连化学物理研究所 General nitrogen is produced superpure nitrogen refining plant and technical process
CN1041333A (en) * 1988-09-24 1990-04-18 中国人民解放军军事医学科学院卫生装备研究所 A kind of making nitrogen by pressure swing adsorption method and equipment
EP0411254A1 (en) * 1989-05-12 1991-02-06 Praxair Technology, Inc. Production of dry, high purity nitrogen

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN85102704A (en) * 1985-04-01 1986-09-24 中国科学院大连化学物理研究所 General nitrogen is produced superpure nitrogen refining plant and technical process
CN1041333A (en) * 1988-09-24 1990-04-18 中国人民解放军军事医学科学院卫生装备研究所 A kind of making nitrogen by pressure swing adsorption method and equipment
EP0411254A1 (en) * 1989-05-12 1991-02-06 Praxair Technology, Inc. Production of dry, high purity nitrogen

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