CN106012379B

CN106012379B - A kind of low emission supercritical fluid dye gigging technique

Info

Publication number: CN106012379B
Application number: CN201610406735.3A
Authority: CN
Inventors: 王威强; 王胜德; 陈银; 曲延鹏; 刘燕
Original assignee: Shandong University
Current assignee: Shandong University
Priority date: 2016-06-06
Filing date: 2016-06-06
Publication date: 2018-01-09
Anticipated expiration: 2036-06-06
Also published as: CN106012379A

Abstract

The present invention relates to textile dyeing field, more particularly to a kind of low emission supercritical fluid dye gigging technique.Implemented by supercritical fluid medium liquefied storage subsystem, two-fold dye device supercritical fluid dyeing subsystem, supercritical fluid deposit subsystem, middle heat accumulation subsystem, filling control subsystem and pipeline；Its processing step includes：1st, dye gigging device A is initialized；2nd, dye gigging device A fills supercritical fluid medium and overcriticalization；3rd, dye gigging device A supercritical fluid dye gigging；4th, dye gigging device B is initialized；5th, dye gigging device A removals pollutant and dye gigging device B fill supercritical fluid medium, overcriticalization and dyeing for the first time；6th, dye gigging device B removals pollutant and dye gigging device A are initialized and filling supercritical fluid medium, overcriticalization and dyeing again；7th, dye gigging device A and dye gigging device B is exchanged, repeats the 6th step.Simple flow of the present invention, equipment investment is small, operating cost is low, time is short, staining efficiency is high, fluid media discharge is small.

Description

A kind of low emission supercritical fluid dye gigging technique

First, technical field

The present invention relates to textile dyeing field, more particularly to a kind of low emission supercritical fluid dye gigging technique.

2nd, technical background

Traditional water dye dyeing can bring substantial amounts of industrial wastewater, and the COD value height of these waste water, ammonia nitrogen discharge capacity are big, Serious destruction is brought to ecological environment, the life and health to resident causes huge threat.Water pollution problems is seriously made About traditional dyeing industrial expansion.According to statistics, the fabric weight of textile printing and dyeing processing and the ratio of water consumption are up to 1:100 ~1:150, national dyeing and printing process water consumption estimation is annual 1600000000 tons.At present, the reuse ratio of the sector production process reclaimed water is very It is low, and sewage disposal and discharge account for production cost ratio and gradually increased.

Supercritical fluid dyeing utilizes supercritical fluid, especially supercritical carbon dioxide, instead of load of the water as dyestuff Body is dyed, and realizes non-aqueous dyeing, so as to fundamentally solve the problems, such as to dye industrial water pollution, there is good open Send out application prospect.

The characteristics of summarizing existing supercritical fluid dyeing technique can be seen that supercritical fluid dyeing and generally include：Storage Supercritical fluid medium, the air being fitted into dyeing with the dyeing installation in dyestuff dissolution system in pollutant and evacuation system, It is super with being filled in dyestuff dissolution system to dyeing by condensing, being pumped, heating and supercritical fluid medium is turned into supercritical fluid Critical fluids, supercritical fluid is set to dye the supercritical fluid dissolving dye for circulating, circulating with being formed in dyestuff dissolution system Expect and upper dye pollutant, stopping circulate and supercritical fluid medium released to supercritical fluid medium stocking system, released Not upper dye dyestuff and supercritical fluid medium are separated in journey, emptying dyeing in dyestuff dissolution system with being less than supercritical fluid medium The supercritical fluid medium of pressure store, pollutant is taken out from dyeing and the dyeing installation in dyestuff dissolution system.It is this super to face The flow of boundary's fluid dyeing technology is complicated, equipment investment is big, operating cost is high, and overcritical medium is condensed, is pumped, is heated as Supercritical fluid and to dyeing with dyestuff dissolution system in fill supercritical fluid process be supercritical fluid dyeing preparation Process, time length, substantially reduces the efficiency of supercritical fluid dyeing, and the popularization for seriously constraining this new technology should With.

It is CN1776086A that China State Intellectual Property Office Patent Office disclosed announcement number on May 24th, 2006, The patent of entitled " supercritical carbon-dioxicle dyeing method of acid fiber by polylactic ", this method solve acid fiber by polylactic without using Water and the technology of the mechanical performance of the dyeing of long period without influenceing fiber can be carried out under the higher temperature more than 110 DEG C ask Topic.The invention is confined to the supercritical CO 2 dyeing of acid fiber by polylactic, can not realize the high quality stains of fabric.Then, It is CN100359091C that China State Intellectual Property Office Patent Office authorized announcement number on January 2nd, 2008, entitled The patent of " process of supercritical CO 2 dyeing ", this method can realize the recovery of non-set dyestuff and realize dyeing The recycling of medium carbon dioxide；China State Intellectual Property Office Patent Office authorized announcement on March 26th, 2014 Number it is CN102817194B, the patent of entitled " a kind of method and apparatus using the static dyeing of supercritical fluid ", the patent A kind of supercritical fluid static state dyeing is provided, dyeing is simple and dyeing installation is easy to clean, and weak point exists Belong to static dyeing in the dyeing, the technical indicator such as its level-dyeing property and dye level is difficult to reach higher level.Above-mentioned three Item patent does not overcome existing supercritical fluid dyeing technological process is complicated, equipment investment is big, operating cost is high, dyes medium to arrange Time long the shortcomings that recycling efficiency low with dyeing medium before high-volume high, dyeing.

3rd, the content of the invention

The purpose of the present invention is the defects of overcoming existing supercritical fluid dyeing technique to exist, there is provided a kind of technological process letter Just, equipment investment is small, operating cost is low, dyes medium low emission, a kind of low row that time is short, staining efficiency is high before dyeing Put supercritical fluid dye gigging technique.

A kind of low emission supercritical fluid dye gigging technique, it is overcritical by supercritical fluid medium liquefied storage subsystem Fluid dyeing subsystem includes：Dye gigging device A and dye gigging device B, rotation, which carries out supercritical fluid medium heating and gasifying, turns into overcritical Fluid, circulation of supercritical fluid, dyestuff dissolving, pollutant move, pollutant are contaminated on dyestuff, and supercritical fluid deposits subsystem, Middle heat accumulation subsystem, fills control subsystem and pipeline is carried out；The process step of the invention is as follows：

1st, dye gigging device A is initialized in supercritical fluid dyeing subsystem：Pollutant is loaded into supercritical fluid dyeing The dye gigging device A of system, install dyestuff additional, and decide whether that installing dyestuff additional helps according to dyestuff and pollutant characteristic and dyeing requirement Solvent, close dye gigging device A；

2nd, dye gigging device A fills supercritical fluid medium and overcriticalization for the first time：Switching supercritical fluid dyeing subsystem follows Circulation journey is to dye gigging device A, by supercritical fluid dyeing demand, by liquid supercritical fluid medium from supercritical fluid medium liquid Change dye gigging device A and its circulation process pipeline that storage subsystem is filled into supercritical fluid dyeing subsystem, make middle storage heater Cooling, the preheating of supercritical fluid medium；Start supercritical fluid dyeing subsystem heating function, arranged using supercritical fluid medium Air in empty supercritical fluid dyeing subsystem in dye gigging device A and its circulation process pipeline, turns into supercritical fluid medium Supercritical fluid；

3rd, supercritical fluid dye gigging：Start pollutant winding mechanism and supercritical fluid dyeing subsystem circulation work( Can, supercritical fluid dissolving dye, upper dye pollutant in cyclic process, dissolved with the super of dyestuff in supercritical fluid dyeing subsystem Critical fluids are realized in the presence of built-in recycle compressor either single external recycle compressor or double external recycle compressors Dissolving dye-above contaminates the circulation of pollutant, while pollutant unreel-go up the reciprocation cycle of dye-winding；

4th, dye gigging device B is initialized in supercritical fluid dyeing subsystem：Dye gigging device A in process 1 is changed to dye gigging device B, Carry out identical operation；

5th, dye gigging device A removals pollutant and dye gigging device B fill supercritical fluid medium, overcriticalization and dyeing for the first time： First, after dye gigging terminates in dye gigging device A, switch valve, make dye gigging device A and supercritical fluid medium liquefied storage subsystem mutual Connection, the overcritical dye matter in dye gigging device A is filled and returns to supercritical fluid medium liquefied storage subsystem, and reaches both pressure Balance, when filling back, heat middle storage heater, the cooling of supercritical fluid medium；Again by complete dyeing dye gigging device A with it is to be dyed Dye gigging device B be interconnected, remaining overcritical dye matter is filled into dye gigging device B in dye gigging device A, and atmospheric valve is first passed through when filling The air in dye gigging device B is emptied, it is equal with dye gigging device A pressure to its pressure to refill dye gigging device B, disconnects dye gigging device A with rolling up Contaminate device B connection；Switch valve is by remaining supercritical fluid contaminates matter in dye gigging device A or the medium of supercritical fluid containing dyestuff is filled into In supercritical fluid medium register, until dye gigging device A equal with pressure in supercritical fluid register, closes supercritical fluid Medium register valve；Remaining supercritical fluid medium in dye gigging device A is emptied by atmospheric valve, carries out unloading cloth afterwards；With Simultaneously, supercritical fluid medium is supplemented into dye gigging device B by supercritical fluid medium liquefied storage subsystem, during supplement, Cool down middle storage heater, the heating of supercritical fluid medium；Start supercritical fluid dyeing subsystem heating function, make overcritical Fluid media turns into supercritical fluid, the supercritical fluid dye gigging process of carry out process 3 in dye gigging device B；

6th, dye gigging device B removals pollutant and dye gigging device A are initialized and filling supercritical fluid medium, overcriticalization again And dyeing：First, dye gigging device A carries out process 1, after terminating, connects supercritical fluid medium register and dye gigging device A, faces super Supercritical fluid medium in boundary's fluid media register is filled into dye gigging device A, and atmospheric valve emptying dye gigging device A is first passed through when filling In air, refill dye gigging device A to its pressure and be equal to supercritical fluid medium register pressure；Concurrently, in dye gigging device B After dye gigging terminates, switch valve, dye gigging device B is set to be interconnected with supercritical fluid medium liquefied storage subsystem, by dye gigging device B In overcritical dye matter fill and return to supercritical fluid medium liquefied storage subsystem, and reach both pressure balances, when filling back, make Middle storage heater heating, the cooling of supercritical fluid medium；It is again that the dye gigging device B and dye gigging device A to be dyed of completing dyeing is mutual Connect, remaining overcritical dye matter is filled into dye gigging device A in dye gigging device B, equal to both pressure, disconnects dye gigging device B with rolling up Contaminate device A connection；Switch valve is by remaining supercritical fluid contaminates matter in dye gigging device B or the medium of supercritical fluid containing dyestuff is filled into In supercritical fluid medium register, until dye gigging device B pressure is equal to supercritical fluid register pressure, supercritical fluid is closed Medium register valve；Remaining supercritical fluid medium in dye gigging device B is emptied by atmospheric valve, carries out unloading cloth afterwards；Most Afterwards, supercritical fluid medium is supplemented into dye gigging device A by supercritical fluid medium liquefied storage subsystem, during supplement, in making Between storage heater cool down, supercritical fluid medium heating；Start supercritical fluid dyeing subsystem heating function, make supercritical fluid Medium turns into supercritical fluid, the supercritical fluid dye gigging process of carry out process 3 in dye gigging device A；

7th, dye gigging device A removals pollutant and dye gigging device B are initialized and filling supercritical fluid medium, overcriticalization again And dyeing：First, dye gigging device B carries out process 4, after terminating, connects supercritical fluid medium register and dye gigging device B, faces super Supercritical fluid medium in boundary's fluid media register is filled into dye gigging device B, and atmospheric valve emptying dye gigging device B is first passed through when filling In air, refill dye gigging device B to its pressure and be equal to supercritical fluid medium register pressure；Concurrently, in dye gigging device A After dye gigging terminates, switch valve, dye gigging device A is set to be interconnected with supercritical fluid medium liquefied storage subsystem, by dye gigging device A In overcritical dye matter fill and return to supercritical fluid medium liquefied storage subsystem, and reach both pressure balances, when filling back, make Middle storage heater heating, the cooling of supercritical fluid medium；It is again that the dye gigging device A and dye gigging device B to be dyed of completing dyeing is mutual Connect, remaining overcritical dye matter is filled into dye gigging device B in dye gigging device A, equal to both pressure, disconnects dye gigging device A with rolling up Contaminate device B connection；Switch valve is by remaining supercritical fluid contaminates matter in dye gigging device A or the medium of supercritical fluid containing dyestuff is filled into In supercritical fluid medium register, until dye gigging device A pressure is equal to supercritical fluid register pressure, supercritical fluid is closed Medium register valve；Remaining supercritical fluid medium in dye gigging device A is emptied by atmospheric valve, carries out unloading cloth afterwards；Most Afterwards, supercritical fluid medium is supplemented into dye gigging device B by supercritical fluid medium liquefied storage subsystem, during supplement, in making Between storage heater cool down, supercritical fluid medium heating；Start supercritical fluid dyeing subsystem heating function, make supercritical fluid Medium turns into supercritical fluid, the supercritical fluid dye gigging process of carry out process 3 in dye gigging device B.

Beneficial effect caused by the present invention：1st, supercritical fluid medium is directly filled into supercritical fluid dye in liquid form Rendering subsystem, pumping operation is saved, save equipment investment, shorten the time of supercritical fluid dyeing, reduce fortune Row expense；2nd, the liquefied storage of supercritical fluid medium and it is combined into one with the separation of excess dye, eliminates independent separation Equipment, equipment investment is reduced, improve utilization rate of equipment and installations；3rd, supercritical dyeing subsystem is discharged using supercritical fluid medium In air, eliminate vaccum-pumping equipment, reduce energy consumption, improve efficiency；4th, the filling of supercritical fluid medium and loopback two During set among storage heater, reduce the condensation power consumption and supercritical fluid of supercritical fluid medium liquefied storage subsystem The heating power consumption of subsystem is dyed, saves operating cost；5th, there is provided dye gigging device A and dye gigging device B, Proximity operation work is improved The utilization rate of overcritical dye matter, shortens total dyeing time, improves efficiency under condition；6th, the deposit of supercritical fluid medium is added Recycling of the device to supercritical fluid medium, the dyeing medium discharge capacity of whole dyeing is low, realizes green production.Always For it, supercritical fluid dye gigging technique provided by the invention, simple flow, equipment investment is small, operating cost is low, dyeing medium Time is short, supercritical fluid dyeing efficiency high before low emission, dyeing.

4th, illustrate

Fig. 1 is the process flow diagram of circulation in the present invention；

Fig. 2 is the process flow diagram of the single external recycle compressor outer circulation of the present invention；

Fig. 3 is the process flow diagram of the double external recycle compressor outer circulations of the present invention；

Fig. 4 is the structural representation of dyeing cycle subsystem dye gigging device in the present invention；

Fig. 5 is the structural representation that subsystem dye gigging device is dyed in outer circulation of the present invention.

Reference：

1st, supercritical fluid medium liquefied storage subsystem C101, supercritical fluid medium storage tank LI101, liquid level gauge PI101, pressure gauge A Va101, safety valve A V101, filling valve V102, stop valve A V103, stop valve B TIC101, temperature control Device A Re101, refrigeration machine E101, condenser 2, supercritical fluid dyeing subsystem D201, dye gigging device A D202, dye gigging device B V201, atmospheric valve A V202, overflow valve A V203, shutoff valve C V204, stop valve D V205, stop valve E V206, stop valve F V207, overflow valve B V208, atmospheric valve B V209, stop valve G V210, stop valve H Va201, safety valve B Va202, safety Valve C M1, motor A M2, motor B M3, motor C M4, motor D C201, external recycle compressor A C202, external circulation pressure Contracting machine B C203, built-in recycle compressor A C204, built-in recycle compressor B FIC201, flow controller A FIC202, stream Amount controller B TIC201, temperature controller B TIC202, temperature controller C PI201, pressure gauge B PI202, pressure gauge C 2-1, filtering Device 2-2, overcritical dye matter hydraulic barrier 2-3, dye cylinder 2-4, heater 2-5, cloth beam A 2-6, overcritical dye matter distribution The overcritical dye matter return channel 3 of device 2-7, cloth beam B 2-8, dye cylinder end cap 2-9, supercritical fluid deposit subsystem V301, Stop valve I Va301, safety valve D C301, overcritical dye matter register PI301, pressure gauge D 4, pipeline 4-1, fluid disengaging Pipe 4-2, fluid outlet pipe 4-3, fluid inlet tubes 5, middle storage heater E501, heat exchanger 6, filling control subsystem V601, regulating valve FIC601, flow controller C.

5th, embodiment

Describe the implementation process of the present invention in detail below in conjunction with the accompanying drawings.

Embodiment one, the low emission supercritical fluid dye gigging technique of built-in recycle compressor.

As shown in figure 1, the low emission supercritical fluid dye gigging technique of built-in recycle compressor passes through supercritical fluid medium Liquefied storage system 1, supercritical fluid dyeing subsystem 2, supercritical fluid deposit subsystem 3, pipeline 4, the and of middle storage heater 5 Filling control subsystem 6 is implemented.

The low emission supercritical fluid dye gigging technique embodiment of built-in recycle compressor is as follows in the present invention：

1st, in supercritical fluid dyeing subsystem 2 dye gigging device A D201 initialization：As shown in figure 4, open dye gigging device A D201, start motor A M1 and pollutant is wound on cloth beam A 2-5, by the free end of pollutant and cloth beam B 2-7 Draw cloth suture；Enough dyestuffs are installed additional in overcritical dye matter distributor 2-6 according to technological requirement, while dissolved according to dyestuff Degree, kinds of fibers, dyeing condition determine whether to install dyestuff cosolvent additional, fine for example with disperse red 60 dyeing terylene Do not install dyestuff cosolvent during dimensional fabric additional, need installation dyestuff cosolvent to enter when dyeing flax or numb fabric with dispersed blue dye Row enzyme ion modification, dyestuff cosolvent polybasic carboxylic acid is added with disperse dark blue S-3BG dyeings pure cotton fabric, uses disperse yellow Need to install dyestuff cosolvent polyethylene glycol additional during E-3RL dyeing polypropylene fabrics；Close dye gigging device A D201.

2nd, dye gigging device A D201 fill supercritical fluid medium and overcriticalization for the first time：As shown in figure 1, according to dye gigging device A D201 completes the amount of the supercritical fluid medium needed for single batch dyeing process, opens stop valve G V209 and filling control subsystem The regulating valve V601 of system 6, by liquid in the supercritical fluid medium storage tank C101 of supercritical fluid medium liquefied storage subsystem 1 Supercritical fluid medium injection dye gigging device A D201 in, open atmospheric valve A V201 during filling, emptying closed after air emptying Valve A V201, flow controller FIC601 control the flow of supercritical fluid medium, while supercritical fluid media stream by measuring Heat exchanger E501 through middle storage heater 5 carries out heat exchange and preheating, and flows into dye gigging device A D201 in liquid form；Wait to surpass Critical fluids medium filling dye gigging device A D201 are completed, and are closed stop valve G V209 and regulating valve V601, are opened dye gigging device A D201 heater 2-4, the supercritical fluid medium in dye gigging device A D201 is heated to the dyeing temperature T of setting₀And Temperature constant state is kept, oil pressure relief P is set according to dye gigging process conditions₀, above-critical state of the supercritical fluid medium into setting And drive supercritical fluid medium excessive in dye gigging device A D201 and enter supercritical fluid medium storage tank through overflow valve A V202 In C101；Overflow valve A V202 make pressure threshold P of the supercritical fluid medium in dye gigging device A D201 all the time in setting₀ Under.

3rd, supercritical fluid dye gigging process：As shown in figure 1, first start motor A M1 and motor B M2, driving cloth beam A 2-5 and cloth beam B 2-7, by controlled motor A M1 and motor B M2, make pollutant past in constant linear velocity and constant-tension Rewinding around；Recycle compressor A C203 built in starting afterwards, the continuous dissolving dye of supercritical fluid forms overcritical dye matter, instant There is the supercritical fluid of dyestuff, it is overcritical to collect inflow by contaminating pollutant on overcritical dye matter distributor 2-6 for overcritical dye matter Dye matter return channel 2-9, and recycle compressor A C203 effects built in warp, return to overcritical dye matter distributor 2-6, are contaminated so as to be in The saturated mode of material, the dynamic circulation process of unsaturated state；Overcritical dye matter distributor 2-6 makes overcritical dye liquor Flow Field Distribution uniform To improve the level-dyeing property of pollutant；Pollutant carries out unreeling in dye gigging device A D201-on dye-winding reciprocation cycle.

4th, in supercritical fluid dyeing subsystem 2 dye gigging device B D202 initialization：As shown in figure 4, open dye gigging device B D202, start motor C M3 and pollutant is wound on cloth beam A 2-5, by the free end of pollutant and cloth beam B 2-7 Draw cloth suture；Enough dyestuffs are installed additional in overcritical dye matter distributor 2-6 according to technological requirement, while dissolved according to dyestuff Degree, kinds of fibers, dyeing condition determine whether to install dyestuff cosolvent additional, fine for example with disperse red 60 dyeing terylene Do not install dyestuff cosolvent during dimensional fabric additional, need installation dyestuff cosolvent to enter when dyeing flax or numb fabric with dispersed blue dye Row enzyme ion modification, dyestuff cosolvent polybasic carboxylic acid is added with disperse dark blue S-3BG dyeings pure cotton fabric, uses disperse yellow Need to install dyestuff cosolvent polyethylene glycol additional during E-3RL dyeing polypropylene fabrics；Close dye gigging device B D202.

5th, dye gigging device A D201 removals pollutants and dye gigging device B D202 fill supercritical fluid medium, overcritical for the first time Change and dye：As shown in figure 1, after dye gigging terminates in dye gigging device A D201, dye gigging device A D201 heater 2-4 is closed, is closed Motor A M1, motor B M2 and built-in recycle compressor A C203, opening stop valve G V209 and regulating valve V601 are closed, makes dye gigging Device A D201 are interconnected with supercritical fluid medium storage tank C101 in supercritical fluid medium liquefied storage subsystem 1, will roll up Overcritical dye matter in dye device A D201, which is filled, returns to supercritical fluid medium liquefied storage subsystem 1, and reaches both pressure and put down Weighing apparatus, regulating valve V601 is closed, when filling back, heat heat exchanger E501, the cooling of supercritical fluid medium；Opening stop valve H V210, the dye gigging device A D201 and dye gigging device B D202 to be dyed that completion is dyed are made to be interconnected, institute in dye gigging device A D201 Surplus overcritical dye matter is filled into dye gigging device B D202, is first passed through when filling in atmospheric valve B V208 emptying dye gigging device B D202 Air, it is equal with dye gigging device A D201 pressure to its pressure to refill dye gigging device B D202, closes stop valve H V210, breaks Uncoiling contaminates device A D201 and dye gigging device B D202 connection；Open stop valve I V301, now dye gigging device A D201 with it is overcritical Contaminate matter register C301 to connect, the overcritical dye matter or the medium of supercritical fluid containing dyestuff in dye gigging device A D201 can enter the excess of imports and face Boundary contaminates matter register C301, after pressure balance, closes stop valve G V209 and stop valve I V301, opens atmospheric valve A V201, overcritical dye matter remaining in dye gigging device A D201 is discharged, close atmospheric valve A V201 afterwards, open dye gigging device A D201, the pollutant contaminated is taken out；Stop valve H V210 and regulating valve V601 are opened, the supercritical fluid medium of liquid is filled Fill in dye gigging device B D202, flow controller FIC601 controls the flow of supercritical fluid medium, while shooting flow by measuring The heat exchanger E501 that body medium flows through middle storage heater 5 carries out heat exchange and preheated, and flows into dye gigging device B in liquid form D202；Treat that supercritical fluid medium filling dye gigging device B D202 are completed, close stop valve H V210 and regulating valve V601, open volume Device B D202 heater 2-4 is contaminated, the supercritical fluid medium in dye gigging device B D202 is heated to the dyeing temperature of setting Spend T₀And temperature constant state is kept, set oil pressure relief P according to dye gigging process conditions₀, super the facing of supercritical fluid medium entrance setting Boundary's state simultaneously drives supercritical fluid medium excessive in dye gigging device B D202 and enters supercritical fluid medium through overflow valve B V207 In storage tank C101；Overflow valve B V207 make pressure threshold of the supercritical fluid medium in dye gigging device B D202 all the time in setting P₀Under；Motor A M1 and motor B M2 are correspondingly replaced by motor C M3 and motor D M4, by built-in recycle compressor A C203 It is replaced by the supercritical fluid dye gigging process of carry out process 3 in built-in recycle compressor B C204, dye gigging device B D202.

6th, dye gigging device B D202 removals pollutants and dye gigging device A D201 are initialized and filling supercritical fluid matchmaker again Matter, overcriticalization and dyeing：As shown in figure 1, dye gigging device A D201 carry out process 1, after terminating, stop valve G V209 are first turned on With stop valve I V301, supercritical fluid medium register C301 and dye gigging device A D201 is connected, supercritical fluid medium is posted Supercritical fluid medium in storage C301 is filled into dye gigging device A D201, opens atmospheric valve A V201, is closed after air emptying Atmospheric valve A V201, supercritical fluid medium register C301 fill supercritical fluid medium to both pressures to dye gigging device A D201 Power is equal, closes stop valve G V209 and stop valve I V301；Concurrently, after dye gigging terminates in dye gigging device B D202, close Closed-book dye device B D202 heater 2-4, closes motor C M3, motor D M4 and built-in recycle compressor B C204, opens and cut Only valve H V210 and regulating valve V601, dye gigging device B D202 are made to face with super in supercritical fluid medium liquefied storage subsystem 1 Boundary fluid media storage tank C101 is interconnected, and the overcritical dye matter in dye gigging device B D202 is filled and returns to supercritical fluid medium liquid Change storage subsystem 1, and reach both pressure balances, close regulating valve V601, when filling back, heat heat exchanger E501, it is super to face Boundary's fluid media cooling；Opening stop valve G V209, make the dye gigging device B D202 that completion is dyed and dye gigging device A to be dyed D201 is interconnected, and remaining overcritical dye matter is filled into dye gigging device A D201 in dye gigging device B D202, fills dye gigging device A D201 is equal with dye gigging device B D202 pressure to its pressure, closes stop valve G V209, disconnects dye gigging device B D202 and dye gigging Device A D201 connection；Stop valve I V301 are opened, now dye gigging device B D202 connect with overcritical dye matter register C301, roll up Overcritical dye matter or the medium of supercritical fluid containing dyestuff in dye device B D202 can enter overcritical dye matter register C301, wait to press After dynamic balance, stop valve H V210 and stop valve I V301 are closed, open atmospheric valve B V208, will be remaining in dye gigging device B D202 Overcritical dye matter discharge, afterwards close atmospheric valve B V208, open dye gigging device B D202, by pollutant contaminate taking-up；Beat Stop valve G V209 and regulating valve V601 are opened, the supercritical fluid medium of liquid is filled in dye gigging device A D201, flow control Device FIC601 controls the flow of supercritical fluid medium by measuring, while supercritical fluid medium flows through changing for middle storage heater 5 Hot device E501 carries out heat exchange and preheated, and flows into dye gigging device A D201 in liquid form；Treat that supercritical fluid medium fills Dye gigging device A D201 are completed, and close stop valve G V209 and regulating valve V601, open dye gigging device A D201 heater 2-4, will Supercritical fluid medium in dye gigging device A D201 is heated to the dyeing temperature T of setting₀And temperature constant state is kept, according to volume Dyeing technique condition setting oil pressure relief P₀, supercritical fluid medium is into the above-critical state set and drives in dye gigging device A D201 Excessive supercritical fluid medium enters in supercritical fluid medium storage tank C101 through overflow valve A V202；Overflow valve A V202 make Pressure threshold P of the supercritical fluid medium all the time in setting in dye gigging device A D201₀Under；Carried out in dye gigging device A D201 The supercritical fluid dye gigging process of journey 3.

7th, dye gigging device A removals pollutant and dye gigging device B are initialized and filling supercritical fluid medium, overcriticalization again And dyeing：As shown in figure 1, dye gigging device B D202 carry out process 4, after terminating, stop valve H V210 and stop valve I are first turned on V301, supercritical fluid medium register C301 and dye gigging device B D202 is connected, by supercritical fluid medium register C301 Supercritical fluid medium be filled into dye gigging device B D202, open atmospheric valve B V208, atmospheric valve B closed after air emptying V208, supercritical fluid medium register C301 fill supercritical fluid medium to pressure phase in both to dye gigging device B D202 Deng closing stop valve H V210 and stop valve I V301；Concurrently, after dye gigging terminates in dye gigging device A D201, volume is closed Device A D201 heater 2-4 is contaminated, closes motor A M1, motor B M2 and built-in recycle compressor A C203, opening stop valve G V209 and regulating valve V601, make dye gigging device A D201 and supercritical fluid matchmaker in supercritical fluid medium liquefied storage subsystem 1 Matter storage tank C101 is interconnected, and the overcritical dye matter in dye gigging device A D201 is filled and returns to supercritical fluid medium liquefied storage System 1, and reach both pressure balances, regulating valve V601 is closed, when filling back, heats heat exchanger E501, supercritical fluid matchmaker Matter cools down；Opening stop valve H V210, the dye gigging device A D201 that completion is dyed are made to be interconnected with dye gigging device B D202 phases to be dyed Logical, remaining overcritical dye matter is filled into dye gigging device B D202 in dye gigging device A D201, fills dye gigging device B D202 to its pressure Power is equal with dye gigging device A D201 pressure, closes stop valve H V210, disconnects dye gigging device A D201 and dye gigging device B D202's Connection；Stop valve I V301 are opened, now dye gigging device A D201 connect with overcritical dye matter register C301, dye gigging device A D201 In overcritical dye matter or the medium of supercritical fluid containing dyestuff can enter overcritical dye matter register C301, after pressure balance, Stop valve G V209 and stop valve I V301 are closed, open atmospheric valve A V201, will be remaining overcritical in dye gigging device A D201 Matter discharge is contaminated, closes atmospheric valve A V201 afterwards, opens dye gigging device A D201, the pollutant contaminated is taken out；Open stop valve H V210 and regulating valve V601, the supercritical fluid medium of liquid is filled in dye gigging device B D202, flow controller FIC601 will The flow of measurement control supercritical fluid medium, while supercritical fluid medium flows through the heat exchanger E501 of middle storage heater 5 and entered Row heat exchange simultaneously preheats, and flows into dye gigging device B D202 in liquid form；Treat supercritical fluid medium filling dye gigging device B D202 is completed, and closes stop valve H V210 and regulating valve V601, dye gigging device B D202 heater 2-4 is opened, by dye gigging device B Supercritical fluid medium in D202 is heated to the dyeing temperature T of setting₀And temperature constant state is kept, according to dye gigging technique bar Part setting oil pressure relief P₀, supercritical fluid medium is into the above-critical state set and drives excessive in dye gigging device B D202 surpass Critical fluids medium enters in supercritical fluid medium storage tank C101 through overflow valve B V207；Overflow valve B V207 make dye gigging device B Pressure threshold P of the supercritical fluid medium all the time in setting in D202₀Under；By the corresponding replacings of motor A M1 and motor B M2 For motor C M3 and motor D M4, built-in recycle compressor A C203 are replaced by built-in recycle compressor B C204, dye gigging device B The supercritical fluid dye gigging process of carry out process 3 in D202.

Dye gigging device A D201 structures in the present embodiment are as shown in figure 4, dye gigging device A D201 main bodys are subject to HTHP Cylinder 2-3 is contaminated, pressure gauge B PI201 and safety valve B Va201 are installed on dye cylinder 2-3；Temperature controller B TIC201 control heater 2-4 with ensure in dyeing course it is overcritical dye matter temperature stabilization；Dye cylinder 2-3 walls are provided with fluid inlet/outlet pipe 4-1 and fluid goes out Mouth pipe 4-2；Overcritical dye matter distributor 2-6 is set in the middle part of dye cylinder 2-3 chambers, it is cavity that it is internal, for containing dyestuff, its circumferential edge A number of distribution hole is provided with close to the side of pollutant, for improving the equal of overcritical dye mass flow field distribution in dyeing course Even property；The dye nearly wall portion of cylinder 2-3 chambers sets overcritical dye matter return channel 2-9；Built-in recycle compressor C203 is along dye gigging device A D201 Heart line is axially mounted, and motor is arranged on outside end cap, and the working-blade of inside installation is arranged on through on the transmission main shaft of end cap； Motor A M1 and motor B M2 be arranged on end cap outside, by power transmission shaft driving inside cloth beam A 2-5, cloth beam B 2-7, Two cloth beams are all drive rolls, by controlled motor A M1 and motor B M2, pollutant is protected during reciprocal winding Hold constant linear velocity and tension force；Overcritical dye matter hydraulic barrier 2-2 is arranged on overcritical dye matter distributor 2-6 end faces, is used In preventing overcritical dye matter from flowing back, prevent to form " short circuit " problem during overcritical dye mass flow is dynamic, improve overcritical dye matter Cycle efficieny.Dye gigging device B D202 have and dye gigging device A D201 identical structures.

Embodiment two, the low emission supercritical fluid dye gigging technique of single external recycle compressor outer circulation.

As shown in Fig. 2 the low emission supercritical fluid dye gigging technique of single external recycle compressor outer circulation pass through it is overcritical Fluid dyeing medium liquefied storage subsystem 1, supercritical fluid dyeing subsystem 2, overcritical dye matter register system 3, pipeline 4, Middle storage heater 5 and flow measurement control subsystem 6 are implemented.

The low emission supercritical fluid dye gigging technique embodiment of single external recycle compressor is as follows in the present invention：

1st, in supercritical fluid dyeing subsystem 2 dye gigging device A D201 initialization：As shown in figure 5, open dye gigging device A D201, start motor A M1 and pollutant is wound on cloth beam A 2-5, by the free end of pollutant and cloth beam B 2-7 Draw cloth suture；Enough dyestuffs are installed additional in overcritical dye matter distributor 2-6 according to technological requirement, while dissolved according to dyestuff Degree, kinds of fibers, dyeing condition determine whether to install dyestuff cosolvent additional, fine for example with disperse red 60 dyeing terylene Do not install dyestuff cosolvent during dimensional fabric additional, need installation dyestuff cosolvent to enter when dyeing flax or numb fabric with dispersed blue dye Row enzyme ion modification, dyestuff cosolvent polybasic carboxylic acid is added with disperse dark blue S-3BG dyeings pure cotton fabric, uses disperse yellow Need to install dyestuff cosolvent polyethylene glycol additional during E-3RL dyeing polypropylene fabrics；Close dye gigging device A D201.

2nd, dye gigging device A D201 fill supercritical fluid medium and overcriticalization for the first time：As shown in Fig. 2 according to dye gigging device A D201 completes the amount of the supercritical fluid medium needed for single batch dyeing process, opens stop valve G V209 and filling control subsystem The regulating valve V601 of system 6, by liquid in the supercritical fluid medium storage tank C101 of supercritical fluid medium liquefied storage subsystem 1 Supercritical fluid medium injection dye gigging device A D201 in, open atmospheric valve A V201 during filling, emptying closed after air emptying Valve A V201, flow controller FIC601 control the flow of supercritical fluid medium, while supercritical fluid media stream by measuring Heat exchanger E501 through middle storage heater 5 carries out heat exchange and preheating, and flows into dye gigging device A D201 in liquid form；Wait to surpass Critical fluids medium filling dye gigging device A D201 are completed, and are closed stop valve G V209 and regulating valve V601, are opened dye gigging device A D201 heater 2-4, the supercritical fluid medium in dye gigging device A D201 is heated to the dyeing temperature T of setting₀And Temperature constant state is kept, oil pressure relief P is set according to dye gigging process conditions₀, above-critical state of the supercritical fluid medium into setting And drive supercritical fluid medium excessive in dye gigging device A D201 and enter supercritical fluid medium storage tank through overflow valve A V202 In C101；Overflow valve A V202 make pressure threshold P of the supercritical fluid medium in dye gigging device A D201 all the time in setting₀ Under.

3rd, supercritical fluid dye gigging process：As shown in Fig. 2 first start motor A M1 and motor B M2, driving cloth beam A 2-5 and cloth beam B 2-7, by controlled motor A M1 and motor B M2, make pollutant past in constant linear velocity and constant-tension Rewinding around；Shutoff valve C V203 and stop valve D V204 is opened, starts external recycle compressor A C201, supercritical fluid is continuous Dissolving dye forms overcritical dye matter, the instant supercritical fluid for having dyestuff, and overcritical dye matter passes through overcritical dye matter distributor Pollutant is contaminated on 2-6, collects and flows into overcritical dye matter return channel 2-9, and is acted on through external recycle compressor A C201, is returned super Critical dye matter distributor 2-6, so as to the saturated mode in dyestuff, the dynamic circulation process of unsaturated state；Overcritical dye matter distribution Device 2-6 makes overcritical dye liquor Flow Field Distribution uniformly to improve the level-dyeing property of pollutant；Pollutant is carried out in dye gigging device A D201 Unreel-go up the reciprocation cycle of dye-winding.

4th, in supercritical fluid dyeing subsystem 2 dye gigging device B D202 initialization：As shown in figure 5, open dye gigging device B D202, start motor C M3 and pollutant is wound on cloth beam A 2-5, by the free end of pollutant and cloth beam B 2-7 Draw cloth suture；Enough dyestuffs are installed additional in overcritical dye matter distributor 2-6 according to technological requirement, while dissolved according to dyestuff Degree, kinds of fibers, dyeing condition determine whether to install dyestuff cosolvent additional, fine for example with disperse red 60 dyeing terylene Do not install dyestuff cosolvent during dimensional fabric additional, need installation dyestuff cosolvent to enter when dyeing flax or numb fabric with dispersed blue dye Row enzyme ion modification, dyestuff cosolvent polybasic carboxylic acid is added with disperse dark blue S-3BG dyeings pure cotton fabric, uses disperse yellow Need to install dyestuff cosolvent polyethylene glycol additional during E-3RL dyeing polypropylene fabrics；Close dye gigging device B D202.

5th, dye gigging device A D201 removals pollutants and dye gigging device B D202 fill supercritical fluid medium, overcritical for the first time Change and dye：As shown in Fig. 2 after dye gigging terminates in dye gigging device A D201, dye gigging device A D201 heater 2-4 is closed, is closed Motor A M1, motor B M2 and external recycle compressor A C201, opening stop valve G V209 and regulating valve V601 are closed, makes dye gigging Device A D201 are interconnected with supercritical fluid medium storage tank C101 in supercritical fluid medium liquefied storage subsystem 1, will roll up Overcritical dye matter in dye device A D201, which is filled, returns to supercritical fluid medium liquefied storage subsystem 1, and reaches both pressure and put down Weighing apparatus, regulating valve V601 is closed, when filling back, heat heat exchanger E501, the cooling of supercritical fluid medium；Opening stop valve H V210, the dye gigging device A D201 and dye gigging device B D202 to be dyed that completion is dyed are made to be interconnected, institute in dye gigging device A D201 Surplus overcritical dye matter is filled into dye gigging device B D202, is first passed through when filling in atmospheric valve B V208 emptying dye gigging device B D202 Air, it is equal with dye gigging device A D201 pressure to its pressure to refill dye gigging device B D202, closes stop valve H V210, breaks Uncoiling contaminates device A D201 and dye gigging device B D202 connection；Open stop valve I V301, now dye gigging device A D201 with it is overcritical Contaminate matter register C301 to connect, the overcritical dye matter or the medium of supercritical fluid containing dyestuff in dye gigging device A D201 can enter the excess of imports and face Boundary contaminates matter register C301, after pressure balance, closes shutoff valve C V203, stop valve D V204, stop valve G V209 and cuts Only valve I V301, atmospheric valve A V201 are opened, overcritical dye matter remaining in dye gigging device A D201 is discharged, close emptying afterwards Valve A V201, dye gigging device A D201 are opened, the pollutant contaminated is taken out；Stop valve H V210 and regulating valve V601 are opened, will The supercritical fluid medium of liquid is filled in dye gigging device B D202, and flow controller FIC601 will be measured and be controlled supercritical fluid matchmaker The flow of matter, while supercritical fluid medium flows through the heat exchanger E501 progress heat exchanges of middle storage heater 5 and preheated, and with Liquid form flows into dye gigging device B D202；Treat that supercritical fluid medium filling dye gigging device B D202 are completed, close stop valve H V210 and regulating valve V601, dye gigging device B D202 heater 2-4 is opened, by the supercritical fluid medium in dye gigging device B D202 It is heated to the dyeing temperature T of setting₀And temperature constant state is kept, set oil pressure relief P according to dye gigging process conditions₀, it is overcritical Fluid media enters the above-critical state of setting and drives supercritical fluid medium excessive in dye gigging device B D202 through overflow valve B V207 enters in supercritical fluid medium storage tank C101；Overflow valve B V207 make the supercritical fluid medium in dye gigging device B D202 All the time the pressure threshold P in setting₀Under；Motor A M1 and motor B M2 are correspondingly replaced by motor C M3 and motor D M4, Shutoff valve C V203 and stop valve D V204 are correspondingly replaced by stop valve E V205 and stop valve F V206, dye gigging device B D202 The supercritical fluid dye gigging process of interior carry out process 3.

6th, dye gigging device B D202 removals pollutants and dye gigging device A D201 are initialized and filling supercritical fluid matchmaker again Matter, overcriticalization and dyeing：As shown in Fig. 2 dye gigging device A D201 carry out process 1, after terminating, stop valve G V209 are first turned on With stop valve I V301, supercritical fluid medium register C301 and dye gigging device A D201 is connected, supercritical fluid medium is posted Supercritical fluid medium in storage C301 is filled into dye gigging device A D201, opens atmospheric valve A V201, is closed after air emptying Atmospheric valve A V201, supercritical fluid medium register C301 fill supercritical fluid medium extremely in both to dye gigging device A D201 Pressure is equal, closes stop valve G V209 and stop valve I V301；Concurrently, after dye gigging terminates in dye gigging device B D202, Dye gigging device B D202 heater 2-4 is closed, closes motor C M3, motor D M4 and external recycle compressor A C201, is opened Stop valve H V210 and regulating valve V601, make dye gigging device B D202 and surpassing in supercritical fluid medium liquefied storage subsystem 1 Critical fluids medium storage tank C101 is interconnected, and the overcritical dye matter in dye gigging device B D202 is filled and returns to supercritical fluid medium Liquefied storage subsystem 1, and reach both pressure balances, regulating valve V601 is closed, when filling back, heats heat exchanger E501, surpasses Critical fluids medium cools down；Opening stop valve G V209, make the dye gigging device B D202 that completion is dyed and dye gigging device A to be dyed D201 is interconnected, and remaining overcritical dye matter is filled into dye gigging device A D201 in dye gigging device B D202, fills dye gigging device A D201 is equal with dye gigging device B D202 pressure to its pressure, closes stop valve G V209, disconnects dye gigging device B D202 and dye gigging Device A D201 connection；Stop valve I V301 are opened, now dye gigging device B D202 connect with overcritical dye matter register C301, roll up Overcritical dye matter or the medium of supercritical fluid containing dyestuff in dye device B D202 can enter overcritical dye matter register C301, wait to press After dynamic balance, stop valve E V205, stop valve F V206, stop valve H V210 and stop valve I V301 are closed, opens atmospheric valve B V208, overcritical dye matter remaining in dye gigging device B D202 is discharged, close atmospheric valve B V208 afterwards, open dye gigging device B D202, the pollutant contaminated is taken out；Stop valve G V209 and regulating valve V601 are opened, the supercritical fluid medium of liquid is filled Fill in dye gigging device A D201, flow controller FIC601 controls the flow of supercritical fluid medium, while shooting flow by measuring The heat exchanger E501 that body medium flows through middle storage heater 5 carries out heat exchange and preheated, and flows into dye gigging device A in liquid form D201；Treat that supercritical fluid medium filling dye gigging device A D201 are completed, close stop valve G V209 and regulating valve V601, open volume Device A D201 heater 2-4 is contaminated, the supercritical fluid medium in dye gigging device A D201 is heated to the dyeing temperature of setting Spend T₀And temperature constant state is kept, set oil pressure relief P according to dye gigging process conditions₀, super the facing of supercritical fluid medium entrance setting Boundary's state simultaneously drives supercritical fluid medium excessive in dye gigging device A D201 and enters supercritical fluid medium through overflow valve A V202 In storage tank C101；Overflow valve A V202 make pressure threshold of the supercritical fluid medium in dye gigging device A D201 all the time in setting P₀Under；The supercritical fluid dye gigging process of carry out process 3 in dye gigging device A D201.

7th, dye gigging device A removals pollutant and dye gigging device B are initialized and filling supercritical fluid medium, overcriticalization again And dyeing：As shown in Fig. 2 dye gigging device B D202 carry out process 4, after terminating, stop valve H V210 and stop valve I are first turned on V301, supercritical fluid medium register C301 and dye gigging device B D202 is connected, by supercritical fluid medium register C301 Supercritical fluid medium be filled into dye gigging device B D202, open atmospheric valve B V208, atmospheric valve B closed after air emptying V208, supercritical fluid medium register C301 fill supercritical fluid medium to pressure phase in both to dye gigging device B D202 Deng closing stop valve H V210 and stop valve I V301；Concurrently, after dye gigging terminates in dye gigging device A D201, volume is closed Device A D201 heater 2-4 is contaminated, closes motor A M1, motor B M2 and external recycle compressor A C201, opening stop valve G V209 and regulating valve V601, make dye gigging device A D201 and supercritical fluid matchmaker in supercritical fluid medium liquefied storage subsystem 1 Matter storage tank C101 is interconnected, and the overcritical dye matter in dye gigging device A D201 is filled and returns to supercritical fluid medium liquefied storage System 1, and reach both pressure balances, regulating valve V601 is closed, when filling back, heats heat exchanger E501, supercritical fluid matchmaker Matter cools down；Opening stop valve H V210, the dye gigging device A D201 that completion is dyed are made to be interconnected with dye gigging device B D202 phases to be dyed Logical, remaining overcritical dye matter is filled into dye gigging device B D202 in dye gigging device A D201, fills dye gigging device B D202 to its pressure Power is equal with dye gigging device A D201 pressure, closes stop valve H V210, disconnects dye gigging device A D201 and dye gigging device B D202's Connection；Stop valve I V301 are opened, now dye gigging device A D201 connect with overcritical dye matter register C301, dye gigging device A D201 In overcritical dye matter or the medium of supercritical fluid containing dyestuff can enter overcritical dye matter register C301, after pressure balance, Shutoff valve C V203, stop valve D V204, stop valve G V209 and stop valve I V301 are closed, opens atmospheric valve A V201, will Remaining overcritical dye matter discharge in dye gigging device A D201, closes atmospheric valve A V201 afterwards, opens dye gigging device A D201, will contaminate Good pollutant takes out；Stop valve H V210 and regulating valve V601 are opened, the supercritical fluid medium of liquid is filled into dye gigging device B In D202, flow controller FIC601 controls the flow of supercritical fluid medium by measuring, while supercritical fluid medium flows through The heat exchanger E501 of middle storage heater 5 carries out heat exchange and preheated, and flows into dye gigging device B D202 in liquid form；Treat super face Boundary fluid media filling dye gigging device B D202 are completed, and are closed stop valve H V210 and regulating valve V601, are opened dye gigging device B D202 Heater 2-4, by the supercritical fluid medium in dye gigging device B D202 be heated to setting dyeing temperature T₀And keep Temperature constant state, oil pressure relief P is set according to dye gigging process conditions₀, above-critical state and drive of the supercritical fluid medium into setting Supercritical fluid medium excessive in dye gigging device B D202 is caught up with to enter supercritical fluid medium storage tank C101 through overflow valve B V207 It is interior；Overflow valve B V207 make pressure threshold P of the supercritical fluid medium in dye gigging device B D202 all the time in setting₀Under；Will Motor A M1 and motor B M2 are correspondingly replaced by motor C M3 and motor D M4, by shutoff valve C V203 and stop valve D V204 couple Stop valve E V205 and stop valve F V206 should be replaced by, the supercritical fluid dye gigging of carry out process 3 in dye gigging device B D202 Journey.

Dye gigging device A D201 structures in the present embodiment are as shown in figure 5, dye gigging device A D201 main bodys are subject to HTHP Cylinder 2-3 is contaminated, pressure gauge B PI201 and safety valve B Va201 are installed on dye cylinder 2-3；Temperature controller B TIC201 control heater 2-4 with ensure in dyeing course it is overcritical dye matter temperature stabilization；Contaminate cylinder 2-3 walls and be provided with fluid inlet/outlet pipe 4-1, fluid issuing Pipe 4-2 and fluid inlet tube 4-3；Overcritical dye matter distributor 2-6 is set in the middle part of dye cylinder 2-3 chambers, it is cavity that it is internal, for containing Dyestuff, its circumference is provided with a number of distribution hole along the side close to pollutant, for improving overcritical dye in dyeing course The uniformity of mass flow field distribution；The dye nearly wall portion of cylinder 2-3 chambers sets overcritical dye matter return channel 2-9；Motor A M1 and motor B M2 peaces Outside end cap, by the cloth beam A 2-5 and cloth beam B 2-7 inside power transmission shaft driving, two cloth beams are all actively Roller, by controlled motor A M1 and motor B M2, make pollutant kept during reciprocal winding constant linear velocity and Power.Dye gigging device B D202 have and dye gigging device A D201 identical structures.

Single external recycle compressor mode has been selected compared with embodiment one, in the present embodiment, can so reduce dye gigging The size of device, more give dye gigging device inner space to pollutant, while be easy to the installation and maintenance of external recycle compressor, But also because overcritical dye matter distributor 2-6 design features make overcritical dye matter be less prone to backflow phenomenon, it is possible to increase super The uniformity that critical dye matter is distributed in dye gigging device interior flow field, the flow for circulating overcritical dye matter are also more prone to control.

Embodiment three, the low emission supercritical fluid dye gigging technique of double external recycle compressor outer circulations.

As shown in figure 3, the low emission supercritical fluid dye gigging technique of double external recycle compressor outer circulations pass through it is overcritical Fluid media liquefied storage subsystem 1, supercritical fluid dyeing subsystem 2, supercritical fluid deposit subsystem 3, pipeline 4, in Between storage heater 5 and filling control subsystem 6 implement.

The low emission supercritical fluid dye gigging technique embodiment of double external recycle compressor outer circulations in the present invention It is as follows：

2nd, dye gigging device A D201 fill supercritical fluid medium and overcriticalization for the first time：As shown in figure 3, according to dye gigging device A D201 completes the amount of the supercritical fluid medium needed for single batch dyeing process, opens stop valve G V209 and filling control subsystem The regulating valve V601 of system 6, by liquid in the supercritical fluid medium storage tank C101 of supercritical fluid medium liquefied storage subsystem 1 Supercritical fluid medium injection dye gigging device A D201 in, open atmospheric valve A V201 during filling, emptying closed after air emptying Valve A V201, flow controller FIC601 control the flow of supercritical fluid medium, while supercritical fluid media stream by measuring Heat exchanger E501 through middle storage heater 5 carries out heat exchange and preheating, and flows into dye gigging device A D201 in liquid form；Wait to surpass Critical fluids medium filling dye gigging device A D201 are completed, and are closed stop valve G V209 and regulating valve V601, are opened dye gigging device A D201 heater 2-4, the supercritical fluid medium in dye gigging device A D201 is heated to the dyeing temperature T of setting₀And Temperature constant state is kept, oil pressure relief P is set according to dye gigging process conditions₀, above-critical state of the supercritical fluid medium into setting And drive supercritical fluid medium excessive in dye gigging device A D201 and enter supercritical fluid medium storage tank through overflow valve A V202 In C101；Overflow valve A V202 make pressure threshold P of the supercritical fluid medium in dye gigging device A D201 all the time in setting₀ Under.

3rd, supercritical fluid dye gigging process：As shown in figure 3, first start motor A M1 and motor B M2, driving cloth beam A 2-5 and cloth beam B 2-7, by controlled motor A M1 and motor B M2, make pollutant past in constant linear velocity and constant-tension Rewinding around；Shutoff valve C V203 and stop valve D V204 is opened, starts external recycle compressor A C201, supercritical fluid is continuous Dissolving dye forms overcritical dye matter, the instant supercritical fluid for having dyestuff, and overcritical dye matter passes through overcritical dye matter distributor Pollutant is contaminated on 2-6, collects and flows into overcritical dye matter return channel 2-9, and is acted on through external recycle compressor A C201, is returned super Critical dye matter distributor 2-6, so as to the saturated mode in dyestuff, the dynamic circulation process of unsaturated state；Overcritical dye matter distribution Device 2-6 makes overcritical dye liquor Flow Field Distribution uniformly to improve the level-dyeing property of pollutant；Pollutant is carried out in dye gigging device A D201 Unreel-go up the reciprocation cycle of dye-winding.

5th, dye gigging device A D201 removals pollutants and dye gigging device B D202 fill supercritical fluid medium, overcritical for the first time Change and dye：As shown in Fig. 2 after dye gigging terminates in dye gigging device A D201, dye gigging device A D201 heater 2-4 is closed, is closed Motor A M1, motor B M2 and external recycle compressor A C201, opening stop valve G V209 and regulating valve V601 are closed, makes dye gigging Device A D201 are interconnected with supercritical fluid medium storage tank C101 in supercritical fluid medium liquefied storage subsystem 1, will roll up Overcritical dye matter in dye device A D201, which is filled, returns to supercritical fluid medium liquefied storage subsystem 1, and reaches both pressure and put down Weighing apparatus, regulating valve V601 is closed, when filling back, heat heat exchanger E501, the cooling of supercritical fluid medium；Opening stop valve H V210, the dye gigging device A D201 and dye gigging device B D202 to be dyed that completion is dyed are made to be interconnected, institute in dye gigging device A D201 Surplus overcritical dye matter is filled into dye gigging device B D202, is first passed through when filling in atmospheric valve B V208 emptying dye gigging device B D202 Air, it is equal with dye gigging device A D201 pressure to its pressure to refill dye gigging device B D202, closes stop valve H V210, breaks Uncoiling contaminates device A D201 and dye gigging device B D202 connection；Open stop valve I V301, now dye gigging device A D201 with it is overcritical Contaminate matter register C301 to connect, the overcritical dye matter or the medium of supercritical fluid containing dyestuff in dye gigging device A D201 can enter the excess of imports and face Boundary contaminates matter register C301, after pressure balance, closes shutoff valve C V203, stop valve D V204, stop valve G V209 and cuts Only valve I V301, atmospheric valve A V201 are opened, overcritical dye matter remaining in dye gigging device A D201 is discharged, close emptying afterwards Valve A V201, dye gigging device A D201 are opened, the pollutant contaminated is taken out；Stop valve H V210 and regulating valve V601 are opened, will The supercritical fluid medium of liquid is filled in dye gigging device B D202, and flow controller FIC601 will be measured and be controlled supercritical fluid matchmaker The flow of matter, while supercritical fluid medium flows through the heat exchanger E501 progress heat exchanges of middle storage heater 5 and preheated, and with Liquid form flows into dye gigging device B D202；Treat that supercritical fluid medium filling dye gigging device B D202 are completed, close stop valve H V210 and regulating valve V601, dye gigging device B D202 heater 2-4 is opened, by the supercritical fluid medium in dye gigging device B D202 It is heated to the dyeing temperature T of setting₀And temperature constant state is kept, set oil pressure relief P according to dye gigging process conditions₀, it is overcritical Fluid media enters the above-critical state of setting and drives supercritical fluid medium excessive in dye gigging device B D202 through overflow valve B V207 enters in supercritical fluid medium storage tank C101；Overflow valve B V207 make the supercritical fluid medium in dye gigging device B D202 All the time the pressure threshold P in setting₀Under；Motor A M1 and motor B M2 are correspondingly replaced by motor C M3 and motor D M4, Shutoff valve C V203 and stop valve D V204 are correspondingly replaced by stop valve E V205 and stop valve F V206, external circulation compression Machine A C201 are replaced by external recycle compressor B C202, the supercritical fluid dye gigging of carry out process 3 in dye gigging device B D202 Journey.

6th, dye gigging device B D202 removals pollutants and dye gigging device A D201 are initialized and filling supercritical fluid matchmaker again Matter, overcriticalization and dyeing：As shown in Fig. 2 dye gigging device A D201 carry out process 1, after terminating, stop valve G V209 are first turned on With stop valve I V301, supercritical fluid medium register C301 and dye gigging device A D201 is connected, supercritical fluid medium is posted Supercritical fluid medium in storage C301 is filled into dye gigging device A D201, opens atmospheric valve A V201, is closed after air emptying Atmospheric valve A V201, supercritical fluid medium register C301 fill supercritical fluid medium extremely in both to dye gigging device A D201 Pressure is equal, closes stop valve G V209 and stop valve I V301；Concurrently, after dye gigging terminates in dye gigging device B D202, Dye gigging device B D202 heater 2-4 is closed, closes motor C M3, motor D M4 and external recycle compressor B C202, is opened Stop valve H V210 and regulating valve V601, make dye gigging device B D202 and surpassing in supercritical fluid medium liquefied storage subsystem 1 Critical fluids medium storage tank C101 is interconnected, and the overcritical dye matter in dye gigging device B D202 is filled and returns to supercritical fluid medium Liquefied storage subsystem 1, and reach both pressure balances, regulating valve V601 is closed, when filling back, heats heat exchanger E501, surpasses Critical fluids medium cools down；Opening stop valve G V209, make the dye gigging device B D202 that completion is dyed and dye gigging device A to be dyed D201 is interconnected, and remaining overcritical dye matter is filled into dye gigging device A D201 in dye gigging device B D202, fills dye gigging device A D201 is equal with dye gigging device B D202 pressure to its pressure, closes stop valve G V209, disconnects dye gigging device B D202 and dye gigging Device A D201 connection；Stop valve I V301 are opened, now dye gigging device B D202 connect with overcritical dye matter register C301, roll up Overcritical dye matter or the medium of supercritical fluid containing dyestuff in dye device B D202 can enter overcritical dye matter register C301, wait to press After dynamic balance, stop valve E V205, stop valve F V206, stop valve H V210 and stop valve I V301 are closed, opens atmospheric valve B V208, overcritical dye matter remaining in dye gigging device B D202 is discharged, close atmospheric valve B V208 afterwards, open dye gigging device B D202, the pollutant contaminated is taken out；Stop valve G V209 and regulating valve V601 are opened, the supercritical fluid medium of liquid is filled Fill in dye gigging device A D201, flow controller FIC601 controls the flow of supercritical fluid medium, while shooting flow by measuring The heat exchanger E501 that body medium flows through middle storage heater 5 carries out heat exchange and preheated, and flows into dye gigging device A in liquid form D201；Treat that supercritical fluid medium filling dye gigging device A D201 are completed, close stop valve G V209 and regulating valve V601, open volume Device A D201 heater 2-4 is contaminated, the supercritical fluid medium in dye gigging device A D201 is heated to the dyeing temperature of setting Spend T₀And temperature constant state is kept, set oil pressure relief P according to dye gigging process conditions₀, super the facing of supercritical fluid medium entrance setting Boundary's state simultaneously drives supercritical fluid medium excessive in dye gigging device A D201 and enters supercritical fluid medium through overflow valve A V202 In storage tank C101；Overflow valve A V202 make pressure threshold of the supercritical fluid medium in dye gigging device A D201 all the time in setting P₀Under；The supercritical fluid dye gigging process of carry out process 3 in dye gigging device A D201.

7th, dye gigging device A removals pollutant and dye gigging device B are initialized and filling supercritical fluid medium, overcriticalization again And dyeing：As shown in Fig. 2 dye gigging device B D202 carry out process 4, after terminating, stop valve H V210 and stop valve I are first turned on V301, supercritical fluid medium register C301 and dye gigging device B D202 is connected, by supercritical fluid medium register C301 Supercritical fluid medium be filled into dye gigging device B D202, open atmospheric valve B V208, atmospheric valve B closed after air emptying V208, supercritical fluid medium register C301 fill supercritical fluid medium to pressure phase in both to dye gigging device B D202 Deng closing stop valve H V210 and stop valve I V301；Concurrently, after dye gigging terminates in dye gigging device A D201, volume is closed Device A D201 heater 2-4 is contaminated, closes motor A M1, motor B M2 and external recycle compressor A C201, opening stop valve G V209 and regulating valve V601, make dye gigging device A D201 and supercritical fluid matchmaker in supercritical fluid medium liquefied storage subsystem 1 Matter storage tank C101 is interconnected, and the overcritical dye matter in dye gigging device A D201 is filled and returns to supercritical fluid medium liquefied storage System 1, and reach both pressure balances, regulating valve V601 is closed, when filling back, heats heat exchanger E501, supercritical fluid matchmaker Matter cools down；Opening stop valve H V210, the dye gigging device A D201 that completion is dyed are made to be interconnected with dye gigging device B D202 phases to be dyed Logical, remaining overcritical dye matter is filled into dye gigging device B D202 in dye gigging device A D201, fills dye gigging device B D202 to its pressure Power is equal with dye gigging device A D201 pressure, closes stop valve H V210, disconnects dye gigging device A D201 and dye gigging device B D202's Connection；Stop valve I V301 are opened, now dye gigging device A D201 connect with overcritical dye matter register C301, dye gigging device A D201 In overcritical dye matter or the medium of supercritical fluid containing dyestuff can enter overcritical dye matter register C301, after pressure balance, Shutoff valve C V203, stop valve D V204, stop valve G V209 and stop valve I V301 are closed, opens atmospheric valve A V201, will Remaining overcritical dye matter discharge in dye gigging device A D201, closes atmospheric valve A V201 afterwards, opens dye gigging device A D201, will contaminate Good pollutant takes out；Stop valve H V210 and regulating valve V601 are opened, the supercritical fluid medium of liquid is filled into dye gigging device B In D202, flow controller FIC601 controls the flow of supercritical fluid medium by measuring, while supercritical fluid medium flows through The heat exchanger E501 of middle storage heater 5 carries out heat exchange and preheated, and flows into dye gigging device B D202 in liquid form；Treat super face Boundary fluid media filling dye gigging device B D202 are completed, and are closed stop valve H V210 and regulating valve V601, are opened dye gigging device B D202 Heater 2-4, by the supercritical fluid medium in dye gigging device B D202 be heated to setting dyeing temperature T₀And keep Temperature constant state, oil pressure relief P is set according to dye gigging process conditions₀, above-critical state and drive of the supercritical fluid medium into setting Supercritical fluid medium excessive in dye gigging device B D202 is caught up with to enter supercritical fluid medium storage tank C101 through overflow valve B V207 It is interior；Overflow valve B V207 make pressure threshold P of the supercritical fluid medium in dye gigging device B D202 all the time in setting₀Under；Will Motor A M1 and motor B M2 are correspondingly replaced by motor C M3 and motor D M4, by shutoff valve C V203 and stop valve D V204 couple Stop valve E V205 and stop valve F V206 should be replaced by, external recycle compressor A C201 are replaced by external recycle compressor The supercritical fluid dye gigging process of carry out process 3 in B C202, dye gigging device B D202.

The mode of double external recycle compressors, two external circulation pressures have been selected compared with embodiment two, in the present embodiment Contracting machine is on independent overcritical dye matter circulation loop, and an external recycle compressor does not influence another volume when breaking down Contaminate the production of device, it is ensured that the continuity of plant running.

Generally speaking, a kind of low emission supercritical fluid dye gigging technique provided by the invention, simple flow, equipment investment It is small, operating cost is low, the low emission of supercritical fluid medium, dyeing before time it is short, supercritical fluid dyeing efficiency high, dyeing Quality is good.

Claims

1. a kind of supercritical fluid dye gigging technique, pass through supercritical fluid medium liquefied storage subsystem, including dye gigging device A and volume Contaminate device B supercritical fluid dyeing subsystem, supercritical fluid deposit subsystem, middle heat accumulation subsystem, filling control subsystem System and pipeline are carried out, it is characterised in that the processing step of supercritical fluid dye gigging technique is as follows：

(1) dye gigging device A is initialized in supercritical fluid dyeing subsystem：Pollutant is loaded into supercritical fluid dyeing subsystem Dye gigging device A, install additional dyestuff, and according to dyestuff and pollutant characteristic and dyeing requirement decide whether install additional dyestuff hydrotropy Agent, close dye gigging device A；

(2) dye gigging device A fills supercritical fluid medium and overcriticalization for the first time：Switch supercritical fluid dyeing subsystem recycle stream Journey, by supercritical fluid dyeing demand, liquid supercritical fluid medium is liquefied from supercritical fluid medium and stored up to dye gigging device A Dye gigging device A and its circulation process pipeline that subsystem is filled into supercritical fluid dyeing subsystem are deposited, cools down middle storage heater, Supercritical fluid medium preheats；Start supercritical fluid dyeing subsystem heating function, emptied using supercritical fluid medium super Air in critical fluids dyeing subsystem in dye gigging device A and its circulation process pipeline, supercritical fluid medium is turned into super and face Boundary's fluid；

(3) supercritical fluid dye gigging：Start pollutant winding mechanism and supercritical fluid dyeing subsystem circulatory function, follow Supercritical fluid dissolving dye, upper dye pollutant during ring, dissolved with the overcritical of dyestuff in supercritical fluid dyeing subsystem Fluid realizes dissolving in the presence of built-in recycle compressor either single external recycle compressor or double external recycle compressors Dyestuff-above contaminates the circulation of pollutant, while pollutant unreel-go up the reciprocation cycle of dye-winding；

(4) dye gigging device B is initialized in supercritical fluid dyeing subsystem：Dye gigging device A in process 1 is changed to dye gigging device B, carried out Identical operation；

(5) dye gigging device A removals pollutant and dye gigging device B fill supercritical fluid medium, overcriticalization and dyeing for the first time：It is first First, after dye gigging terminates in dye gigging device A, switch valve, dye gigging device A is made mutually to be interconnected with supercritical fluid medium liquefied storage subsystem It is logical, the overcritical dye matter in dye gigging device A is filled and returns to supercritical fluid medium liquefied storage subsystem, and reaches both pressure and puts down Weighing apparatus, when filling back, heat middle storage heater, the cooling of supercritical fluid medium；Again by complete dyeing dye gigging device A with it is to be dyed Dye gigging device B is interconnected, and remaining overcritical dye matter is filled into dye gigging device B in dye gigging device A, and atmospheric valve row is first passed through when filling Air in blank coil dye device B, it is equal with dye gigging device A pressure to its pressure to refill dye gigging device B, disconnection dye gigging device A and dye gigging Device B connection；Remaining supercritical fluid dye matter or the medium of supercritical fluid containing dyestuff in dye gigging device A are filled into super by switch valve In critical fluids medium register, until dye gigging device A equal with pressure in supercritical fluid register, closes supercritical fluid matchmaker Matter register valve；Remaining supercritical fluid medium in dye gigging device A is emptied by atmospheric valve, carries out unloading cloth afterwards；Therewith Meanwhile supercritical fluid medium is supplemented into dye gigging device B by supercritical fluid medium liquefied storage subsystem, during supplement, make Middle storage heater cooling, the heating of supercritical fluid medium；Start supercritical fluid dyeing subsystem heating function, make shooting flow Body medium turns into supercritical fluid, the supercritical fluid dye gigging process of carry out process 3 in dye gigging device B；

(6) dye gigging device B removals pollutant and dye gigging device A initialize again with filling supercritical fluid medium, overcriticalization and Dyeing：First, dye gigging device A carries out process 1, after terminating, connects supercritical fluid medium register and dye gigging device A, will be overcritical Supercritical fluid medium in fluid media register is filled into dye gigging device A, is first passed through when filling in atmospheric valve emptying dye gigging device A Air, refill dye gigging device A to its pressure and be equal to supercritical fluid medium register pressure；Concurrently, rolled up in dye gigging device B After dye terminates, switch valve, dye gigging device B is set to be interconnected with supercritical fluid medium liquefied storage subsystem, by dye gigging device B Overcritical dye matter fill and return to supercritical fluid medium liquefied storage subsystem, and reach both pressure balances, when filling back, in making Between storage heater heat, supercritical fluid medium cooling；The dye gigging device B for completing dyeing is interconnected with dye gigging device A phases to be dyed again Logical, remaining overcritical dye matter is filled into dye gigging device A in dye gigging device B, equal to both pressure, disconnects dye gigging device B and dye gigging Device A connection；Remaining supercritical fluid dye matter or the medium of supercritical fluid containing dyestuff in dye gigging device B are filled into super by switch valve In critical fluids medium register, until dye gigging device B pressure is equal to supercritical fluid register pressure, supercritical fluid matchmaker is closed Matter register valve；Remaining supercritical fluid medium in dye gigging device B is emptied by atmospheric valve, carries out unloading cloth afterwards；Finally, Supercritical fluid medium is supplemented into dye gigging device A by supercritical fluid medium liquefied storage subsystem, during supplement, makes middle storage Hot device cooling, the heating of supercritical fluid medium；Start supercritical fluid dyeing subsystem heating function, make supercritical fluid medium As supercritical fluid, the supercritical fluid dye gigging process of carry out process 3 in dye gigging device A；

(7) dye gigging device A removals pollutant and dye gigging device B initialize again with filling supercritical fluid medium, overcriticalization and Dyeing：First, dye gigging device B carries out process 4, after terminating, connects supercritical fluid medium register and dye gigging device B, will be overcritical Supercritical fluid medium in fluid media register is filled into dye gigging device B, is first passed through when filling in atmospheric valve emptying dye gigging device B Air, refill dye gigging device B to its pressure and be equal to supercritical fluid medium register pressure；Concurrently, rolled up in dye gigging device A After dye terminates, switch valve, dye gigging device A is set to be interconnected with supercritical fluid medium liquefied storage subsystem, by dye gigging device A Overcritical dye matter fill and return to supercritical fluid medium liquefied storage subsystem, and reach both pressure balances, when filling back, in making Between storage heater heat, supercritical fluid medium cooling；The dye gigging device A for completing dyeing is interconnected with dye gigging device B phases to be dyed again Logical, remaining overcritical dye matter is filled into dye gigging device B in dye gigging device A, equal to both pressure, disconnects dye gigging device A and dye gigging Device B connection；Remaining supercritical fluid dye matter or the medium of supercritical fluid containing dyestuff in dye gigging device A are filled into super by switch valve In critical fluids medium register, until dye gigging device A pressure is equal to supercritical fluid register pressure, supercritical fluid matchmaker is closed Matter register valve；Remaining supercritical fluid medium in dye gigging device A is emptied by atmospheric valve, carries out unloading cloth afterwards；Finally, Supercritical fluid medium is supplemented into dye gigging device B by supercritical fluid medium liquefied storage subsystem, during supplement, makes middle storage Hot device cooling, the heating of supercritical fluid medium；Start supercritical fluid dyeing subsystem heating function, make supercritical fluid medium As supercritical fluid, the supercritical fluid dye gigging process of carry out process 3 in dye gigging device B.