CN106676796B - A kind of flax roving supercritical CO2Anhydrous bleaching device and its method for bleaching - Google Patents

A kind of flax roving supercritical CO2Anhydrous bleaching device and its method for bleaching Download PDF

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CN106676796B
CN106676796B CN201611039618.4A CN201611039618A CN106676796B CN 106676796 B CN106676796 B CN 106676796B CN 201611039618 A CN201611039618 A CN 201611039618A CN 106676796 B CN106676796 B CN 106676796B
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bleaching
kettle
gas
cosolvent
liquid
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CN106676796A (en
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郑来久
张娟
高世会
郑环达
闫俊
韩益桐
吴劲松
李飞霞
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Yixing City Shunshine Linen Textile Co ltd
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Dalian Polytechnic University
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Abstract

The invention discloses a kind of flax roving supercritical COs2Anhydrous bleaching device and its method for bleaching improve the structure of blender and separator in prior art basis, and flax roving is successively placed in bleaching kettle by when bleaching, with H2O2Solution is cosolvent, reaches supercritical CO2When state, in 50-150 DEG C of temperature, pressure 8-30MPa, CO230-150min is bleached under the conditions of fluid flow 10-50g/min.Flax roving whiteness 40-75%, rate of weight loss 7-10%, residual gum content 7-12.5% after bleaching, broken filament intensity 5-12cN/dtex, elongation at break 5-8%.The present invention utilizes CO2It is produced instead of the bleaching that cleans that aqueous medium realizes flax roving, bleaching overall process is pollution-free, zero-emission, embodies the modern life theory of fashion bast fibre spinning, green bast fibre spinning.

Description

Supercritical CO of flax roving2Anhydrous bleaching device and bleaching method thereof
Technical Field
The invention relates to supercritical CO2A fluid anhydrous bleaching technology, in particular to a supercritical CO of flax roving2An anhydrous bleaching device and a bleaching method thereof.
Background
The flax fiber is the high-quality plant fiber used by human beings at the earliest and accounts for 1.5 percent of the total amount of the natural fiber. The chemical components of the flax fiber mainly comprise cellulose, hemicellulose, pectin, lignin, wax, nitrogen-containing substances and the like, wherein the hemicellulose, the lignin and the pectin are difficult to remove, and the crystallinity and the orientation degree of flax fiber molecules are high, so that the flax fiber molecules are easy to influence the extensibility, elasticity, bundling property, softness and crimpability of the fibers, and inconvenience is brought to the spinning and weaving process of the flax fibers. Therefore, bleaching of flax roving has been a problem of concern in the linen industry. For many years, many research works are based on solving the problem, and people do not begin to research the bleaching process of the flax roving until the later 20 th century 50 years, and wet spinning is carried out after the bleaching of the roving, so that the concomitant product is fully swelled, partial impurities are removed, and the spinnability of the fiber is improved. At the end of the 50 s, the flax roving bleaching technology was successfully developed in China; the flax roving bleaching equipment was substantially perfect at the end of the 70 s.
In the traditional bleaching process of the flax roving, water is mainly used as a medium, and the steps of alkali boiling, sodium chlorite bleaching, water washing, hydrogen peroxide bleaching, water washing, acid washing and water washing are sequentially carried out to remove hemicellulose, lignin and pectin in fibers, so that the requirements on the strength and whiteness of the flax roving fibers in the spinning process are finally met. After the flax roving is bleached, substances among partial bonding fibers are removed, the connection among the fibers is weakened, the splitting degree of the flax fibers is improved, and the spinnability of the flax fibers is improved. However, the traditional bleaching process of the flax roving has the defects of high water and energy consumption, long process flow, high economic cost and the like. Meanwhile, after bleaching production, the discharged sewage contains a large amount of sodium chlorite, sodium carbonate, hydrogen peroxide and other auxiliary agents, which brings serious pollution to the environment.
A substance is converted to a supercritical fluid when its temperature and pressure are above its critical temperature and critical pressure at normal conditions. In the supercritical state, small changes in pressure and temperature can cause significant differences in fluid density and manifest as changes in fluid solubility, making supercritical fluids extremely valuable for applications. Since 1978 the first international conference of supercritical fluid extraction held by western Essen, the supercritical fluid extraction technology has been widely applied to the fields of medicine, chemical industry, food, environmental protection and the like for more than 30 years. The supercritical fluid extraction technology is that under the condition of not changing chemical composition, the supercritical fluid is contacted with separation substance by utilizing the relation of dissolving capacity and density of the supercritical fluid, so that the separation substance can selectively extract components with polarity, boiling point and molecular weight in turn, and then the extraction separation purpose is realized by utilizing the influence of temperature and pressure on the dissolving capacity of the supercritical fluid. Among the substances commonly used, CO2The supercritical fluid is the most widely applied supercritical fluid due to the characteristics of no toxicity, no harm, no combustion, chemical inertness, unique quadrupole structure, low critical temperature (31.1 ℃) and critical pressure (7.27MPa) and the like.
In order to solve the problems of high pollution and high energy consumption in the bleaching process of the flax roving, the invention provides supercritical CO of the flax roving2An anhydrous bleaching process.
Disclosure of Invention
In order to solve the problems of high pollution and high energy consumption in the bleaching process of the flax roving, the invention provides supercritical CO for the flax roving2Anhydrous bleaching device and bleaching method thereof, using CO2The method realizes the clean bleaching production of the flax roving instead of an aqueous medium, and has great significance for the technical transformation and upgrading of the flax spinning industry.
Supercritical CO of flax roving2An anhydrous bleaching plant comprising a structural unit CO2Storage tank, filter, blender and booster pumpThe device comprises a preheater, a heater, a bleaching kettle, a separation kettle, a cosolvent tank, a liquid delivery pump and a magnetic circulating pump, wherein the CO is introduced into the bleaching kettle2The storage tank, the filter, the blender, the booster pump, the preheater, the bleaching kettle and the separation kettle are sequentially connected through a pipeline, the cosolvent tank is connected with the blender after being connected with the liquid delivery pump through a pipeline, and the heater is communicated with the upstream and the downstream of the bleaching kettle through a pipeline and used for heating materials in the bleaching kettle; the magnetic circulating pump is communicated with the upstream and downstream of the bleaching kettle through a pipeline and is used for circulating materials in the bleaching kettle; it is characterized in that the preparation method is characterized in that,
the structural unit of the blender is as follows:
from CO2Inlet, CO2The outlet, the cosolvent inlet, the cosolvent passage, the pinhole conveying pipe inlet, the pinhole conveying pipe outlet, the pinhole conveying pipe and the gas-liquid mixing passage; the gas-liquid mixing channel is provided with a cavity with a cylindrical structure, a plurality of pinhole conveying pipes are uniformly distributed on the upper bottom surface and the lower bottom surface of the gas-liquid mixing channel respectively, the outer side end of each pinhole conveying pipe is communicated with the flat cylindrical cosolvent channel, and the center of the bottom surface of the cosolvent channel facing to the outer side is provided with a cosolvent inlet; CO is symmetrically arranged on the side wall of the cylindrical structure of the gas-liquid mixing channel2Inlet, CO2An outlet; the pinhole delivery pipes are arranged on the gas-liquid mixing channel in a mode of being crossed at the opposite positions in the vertical direction so as to keep the cosolvent to be uniformly injected along the gas-liquid mixing channel and realize the CO2And complete mixing of the co-solvent.
The separation kettle structure unit:
the gas-liquid mixer comprises a cylinder body and a top cover, wherein the cylinder body and the top cover are connected through a bolt, the cylinder body is provided with a gas-liquid mixture inlet, a liquid outlet and a gas outlet I, the gas-liquid mixture inlet is positioned on the side wall of the cylinder body, the liquid outlet is arranged below the cylinder body, and the gas outlet I is arranged above the cylinder body; fixedly connected with spiral separator in the barrel, spiral separator includes spiral pipe, spiral pipe entry end and spiral pipe exit end from top to bottom, the spiral pipe entry end is connected with the gas-liquid mixture entry, the spiral pipe exit end is connected with the liquid outlet, the sealed filter sieve that is provided with on the port inner wall of spiral pipe exit end, gas outlet II has been seted up on the spiral pipe exit end, gas outlet II is located filter sieve and spiral pipe between.
Specifically, for the bleaching device described above, wherein the spiral tube is filled with a filler, the filler is silica gel or polystyrene, and the particle size of the filler is 1 to 10 μm.
Specifically, in the bleaching apparatus described above, the particle size of the filler in the spiral tube decreases gradually from the inlet of the gas-liquid mixture to the gas outlet ii.
Specifically, with the bleaching apparatus described above, wherein the spiral separator is detachably mounted in the cylinder of the separation vessel.
Specifically, in the bleaching apparatus described above, at least one of the separation tanks is connected in series by a pipe.
Specifically, in the bleaching apparatus described above, the pinhole ducts of the blender are arranged in the gas-liquid mixing passage in a manner of being staggered in the vertical direction relative to each other.
The invention also discloses a bleaching method of the flax roving, which adopts the flax roving supercritical CO2The anhydrous bleaching device carries out bleaching.
In particular, the method uses 30% of H2O2The solution is a bleaching agent. The bleaching conditions of the bleaching method are as follows: supercritical CO2The fluid flow rate is 10-50g/min, the internal temperature of the bleaching kettle is 50-150 ℃, the pressure is 8-30MPa, and the bleaching time is 30-150 min.
The equipment units with the same function in the supercritical carbon dioxide fluid anhydrous bleaching equipment can comprise a plurality of equipment units, such as a plurality of booster pumps and heaters, a plurality of bleaching kettles, a plurality of separators and the like. The skilled person can set the process according to the requirements of the throughput.
Specifically, for the bleaching device, two separation kettles are connected in series through a pipeline to form a multi-stage separation kettle; each separation kettle is internally provided with a detachable spiral tube type separator to increase the separation area, and fine separation is carried out in sequence according to the molecular size of the extract.
Specifically, the bleaching device is composed of two bleaching kettles which are connected in parallel through a pipeline.
H in cosolvent tank2O2The CO-solvent is injected into the CO-solvent inlet of the blender under the action of the liquid delivery pump, enters the inlet of the pinhole delivery pipe through the CO-solvent channel, flows out of the outlet of the pinhole delivery pipe through the pinhole delivery pipe, and is mixed with CO in the gas-liquid mixing channel2The mixture is fully mixed and injected into the bleaching kettle and enters a supercritical state under the action of a preheater. Supercritical CO with dissolved cosolvent2Entering a bleaching kettle, putting the flax roving into the bleaching kettle, and adding H2O2The solution is a cosolvent to achieve supercritical CO2In the state, CO is at 50-150 deg.C and 8-30MPa2The flow rate of the fluid is 10-50g/min, and the flax roving is circularly bleached for 30-150min by using a magnetic circulating pump under the condition. After bleaching, keeping the pressure at 3MPa and the temperature at 30 ℃ for CO2Recovering the fluid to obtain bleached flax roving; the whiteness of the bleached flax roving is 40-75%, the weight loss rate is 7-10%, the residual gum rate is 7-12.5%, the breaking strength of single fibers is 5-12cN/dtex, and the breaking elongation is 5-8%. The invention utilizes CO2The method has the advantages that the method replaces an aqueous medium to realize the clean bleaching production of the flax roving, the whole bleaching process is pollution-free and zero-emission, and the modern life concept of fashion flax spinning and green flax spinning is reflected.
The flax roving supercritical CO2The anhydrous bleaching method comprises the following process flows: placing the flax roving in the supercritical CO described above2In a bleaching kettle; starting the refrigeration system when CO2The pressure of the storage tank is reduced to 4.0MPa, and CO is generated2When the liquid level of the storage tank rises to 400mm, CO starts to be introduced into the bleaching kettle2To make CO2The flow rate of the fluid is 10-50 g/min;
in particular, CO2CO output from storage tank2The fluid, filtered through a filter, was injected into the interior of the blender via a high pressure pump. The co-solvent in the co-solvent tank was injected into the blender via a liquid transfer pump. CO22After being uniformly mixed with the cosolvent in the blender, the mixture enters a preheater through a booster pump for primary heating so as to increase the mixing effect; and then the mixture enters a heater for secondary temperature rise to meet the requirement of bleaching conditions. Supercritical CO2The fluid carrying the cosolvent enters two or more bleaching kettles which are arranged in parallel to carry out bleaching on the flax roving. And drives the supercritical CO under the action of the magnetic circulating pump2The fluid circularly flows between the bleaching kettles to finish the bleaching production. Supercritical CO with cosolvent after bleaching2The fluid is subjected to multistage separation in two or more separation kettles which are arranged in series in sequence, and supercritical CO is obtained2Gasification to CO2The gas and the cosolvent are liquefied into liquid and stored in the separation kettle. CO22The gas is filtered by a purifier and then recycled into CO2And (4) storing the tank for carrying out the next bleaching production. The evaporator is connected with CO2Storage tank and condenser to balance CO2The pressure in the storage tank.
In particular, CO as described above2The process flow of the cosolvent in the blender is as follows:
h in the cosolvent tank2O2The CO-solvent is injected into the CO-solvent inlet of the blender under the action of the liquid delivery pump, enters the inlet of the pinhole delivery pipe through the CO-solvent channel, flows out of the outlet of the pinhole delivery pipe through the pinhole delivery pipe, and is mixed with CO in the gas-liquid mixing channel2The mixture is fully mixed and injected into the bleaching kettle and enters a supercritical state under the action of a preheater. Supercritical CO with dissolved cosolvent2Entering bleaching kettle to make the internal temperature of bleaching kettle be 50-150 deg.C and pressureUnder the condition of 8-30MPa, performing flax roving circulating bleaching by using a magnetic circulating pump, wherein the bleaching time is 30-150 min; after bleaching, keeping the pressure at 3MPa and the temperature at 30 ℃ for CO2And recovering the fluid to obtain the bleached flax roving.
The invention has the beneficial effects that:
1. compared with the traditional chemical bleaching method, the separation kettle is detachably fixed with a spiral separator to increase the separation area, and the fillers are filled according to the sizes of different particles, so that the aim of sequentially and finely separating the extract according to the molecular sizes of the extract is further fulfilled2And complete mixing of the co-solvent.
2. The bleaching method of the invention usually needs CO for producing one kilogram of ramie2Flow rate 0.1-1kg, requiring H2O20-0.2kg of solution, the bleaching time is 30-150min, the whiteness of the bleached flax roving is 45-75%, the weight loss rate of the roving is 5-10%, the residual gum rate is 8-12%, the breaking strength of a single fiber is 6-12cN/dtex, and the breaking elongation is 4-7%; the invention relates to a supercritical CO of flax roving2The whole process of the fluid bleaching method is pollution-free and zero-emission, and the modern life concept of fashion linen spinning and green linen spinning is reflected.
Drawings
FIG. 1. flax roving supercritical CO2A fluid bleaching process schematic;
1.CO2the system comprises a storage tank, a blender 2, a bleaching kettle 3, a separation kettle 4, a filter 5, a preheater 6, a liquid delivery pump 7, a cosolvent tank 8, a booster pump 9, a heater 10 and a magnetic circulating pump 11;
FIG. 2 is a schematic diagram of a blender;
22、CO2inlet, 23, CO2Outlet, 24, cosolvent inlet, 25, cosolvent passage, 26, pinhole conveying pipe inlet, 27, pinhole conveying pipe outlet, 28, pinhole conveying pipe, 29 and gas-liquid mixing passage;
FIG. 3 is a schematic view of a spiral separator;
41. the device comprises a cylinder body 42, a top cover 411, a gas-liquid mixture inlet 412, a liquid outlet 413, a gas outlet I, a gas outlet 43, a spiral separator 431, a spiral pipe inlet end 432, a spiral pipe 433, a spiral pipe outlet end 434, a filtering sieve plate 435 and a gas outlet II.
FIG. 4 is a multi-stage separation kettle formed by connecting two separation kettles in series through a pipeline;
FIG. 5, two bleaching kettles are connected in parallel through a pipeline.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
The test methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
The whiteness is tested according to GB/T17644-; the single fiber breaking strength and the elongation at break are tested according to GB/T5886-86, Ramie single fiber breaking strength test method.
Example 1
The following detailed description of the invention refers to the accompanying drawings. The structure of the bleaching kettle used in the following examples is a supercritical carbon dioxide cheese dyeing kettle disclosed in chinese patent publication No. CN102787459A, such as the dyeing kettle structure described in example 1 of the publication.
The invention relates to a supercritical CO of flax roving2Bleaching device:
supercritical CO of flax roving2An anhydrous bleaching plant comprising a structural unit CO2The device comprises a storage tank 1, a filter 5, a blender 2, a booster pump 9, a preheater 6, a heater 10, a bleaching kettle 3, a separation kettle 4, a cosolvent tank 8, a liquid delivery pump 7 and a magnetic circulation pump 11, wherein the CO2 storage tank 1, the filter 5, the blender 2, the booster pump 9, the preheater 6, the bleaching kettle 3 and the separation kettle 4 are sequentially connected through a pipeline, the cosolvent tank 8 is connected with the liquid delivery pump 7 through a pipeline and then is connected with the blender 2, and the heater 10 is communicated with the bleaching kettle 3 through a pipeline in an upstream-downstream mode and is used for heating materials in the bleaching kettle 3; the magnetic circulating pump 11 is communicated with the upstream and downstream of the bleaching kettle 3 through a pipeline and is used for circulating materials in the bleaching kettle 3; wherein,
the structural unit of the blender 2 is as follows:
from CO2Inlet, CO2The outlet, the cosolvent inlet, the cosolvent passage, the pinhole conveying pipe inlet, the pinhole conveying pipe outlet, the pinhole conveying pipe and the gas-liquid mixing passage; the gas-liquid mixing channel is provided with a cavity with a cylindrical structure, a plurality of pinhole conveying pipes are uniformly distributed on the upper bottom surface and the lower bottom surface of the gas-liquid mixing channel respectively, the outer side end of each pinhole conveying pipe is communicated with the flat cylindrical cosolvent channel, and the center of the bottom surface of the cosolvent channel facing to the outer side is provided with a cosolvent inlet; CO is symmetrically arranged on the side wall of the cylindrical structure of the gas-liquid mixing channel2Inlet, CO2An outlet; the arrangement mode of the pinhole conveying pipes on the blender 2 on the gas-liquid mixing channel is that the pinhole conveying pipes are arranged in a crossed mode at the opposite positions in the vertical direction.
The separation kettle structure unit is as follows:
the gas-liquid separator comprises a cylinder body 41 and a top cover 42, wherein the cylinder body 41 is connected with the top cover 42 through a bolt, a gas-liquid mixture inlet 411, a liquid outlet 412 and a gas outlet I413 are formed in the cylinder body 41, the gas-liquid mixture inlet 411 is located on the side wall of the cylinder body 41, the liquid outlet 412 is arranged below the cylinder body 41, and the gas outlet I413 is arranged above the cylinder body 41; fixedly connected with spiral separator 43 in barrel 41, spiral separator 43 from top to bottom includes spiral pipe 432, spiral pipe entry end 431 and spiral pipe exit end 433, spiral pipe entry end 431 is connected with gas-liquid mixture entry 411, spiral pipe exit end 433 is connected with liquid outlet 412, sealed being provided with on the port inner wall of spiral pipe exit end 433 filters sieve 434, gas outlet II 435 has been seted up on spiral pipe exit end 433, gas outlet II 435 is located between filtration sieve 434 and the spiral pipe 432.
The spiral tube 432 is filled with a filler which is silica gel or polystyrene, and the particle size of the filler is 1-10 μm. The particle size of the packing gradually decreases from the gas-liquid mixture inlet 411 to the gas outlet II 435. The spiral separator 43 is detachably mounted in the cylinder 41 of the separation vessel.
Utilize flax roving supercritical CO of above-mentioned device2The bleaching method comprises the following bleaching working processes:
(1) internal circulation bleaching:
firstly, flax roving bobbins are sequentially connected and sleeved in a bleaching kettle 3, and H is used2O2The solution is a cosolvent and is placed in a cosolvent tank 8.
Starting a refrigeration system, when the pressure of a CO2 storage tank 1 is reduced to 4.0MPa, the liquid level of a CO2 storage tank 1 is increased to 400mm, and introducing CO into a bleaching kettle 32To make CO2The flow rate of the fluid is 10-50 g/min; liquid CO2When flowing out of the CO2 storage tank 1, the CO is filtered by a filter 5 to remove impurities which may be contained.
H in cosolvent tank 82O2The solution is injected into the co-solvent inlet of the blender 2 under the action of the liquid transfer pump 724 and through co-solvent passageway 25 into pinhole delivery tube inlet 26 and out pinhole delivery tube outlet 27 through pinhole delivery tube 28. CO2 enters blender 2 through CO2 inlet 22 under the action of high pressure pump and is fully mixed with the cosolvent in gas-liquid mixing channel 29. CO homogeneously dissolved with CO-solvent2CO from blender 22The outlet flows out and then enters a supercritical state under the action of the preheater 6. Supercritical CO with dissolved cosolvent2Entering a bleaching kettle 3, leading the internal temperature of the bleaching kettle 3 to be 50-150 ℃ and the pressure to be 8-30MPa, and circularly bleaching flax roving by using a magnetic circulating pump 11 under the condition for 30-150 min; after bleaching, keeping the pressure at 3MPa and the temperature at 30 ℃ for CO2Recovering the fluid to obtain bleached flax roving;
(2) supercritical CO2The fluid flows into the bleaching kettle 3, permeates and diffuses from bottom to top towards the flax cheese on the bleaching kettle and then flows out; under the action of the magnetic circulating pump 11, CO2The fluid enters the bleaching kettle 3 again, the internal temperature of the bleaching kettle 3 is kept at 50-150 ℃, the pressure is 8-30MPa, and the bleaching circulation is realized for 30-150min by using the magnetic circulating pump 11 under the condition; the heat loss of the bleaching process is compensated by the heater 10. External circulation bleaching:
sequentially connecting and sleeving flax roving bobbins in a bleaching kettle 3, and passing the flax roving through supercritical CO2After the fluid is bleached for 20-40min, the running direction of the fluid is changed, and CO is generated at the time2The fluid enters through the top gas channel of the bleaching kettle 3; the flax cone yarns on the flax cone yarns flow out after being permeated and diffused from top to bottom; under the action of the magnetic circulating pump 11, CO2The fluid enters the bleaching kettle 3 again to realize external circulation bleaching.
The heat loss of the bleaching process is compensated by the heater 10. After the bleaching process is completed, the high-pressure pump and the magnetic circulation pump 11 are turned off. Supercritical CO in bleaching kettle 32The fluid enters a multistage separation kettle 4, enters a spiral separator 43 in the separation kettle through a gas-liquid mixture inlet 411 of the separation kettle and an inlet of the spiral separator 43, and is kept at 3MPa and 2 MPa under the action of gradual change type filling materials in the separatorAt 0 ℃ the bleaching product is brought into contact with CO2Completely separating gas; bleaching products can sequentially flow out of the spiral separator 43 according to the molecular weight when passing through fillers with different particle sizes, and a filtering sieve plate 434 arranged in the spiral separator 43 can filter solid products such as fibers, so that the separation effect is improved. The liquid bleaching product separated by the spiral separator 43 can be discharged through a liquid outlet 412 at the bottom of the separation kettle cylinder 41, and is further purified and then recycled; liquid CO after passing through the spiral separator 432Conversion to gaseous CO2Gaseous CO2Flows out through a gas outlet II 435 of the spiral separator 43, passes through a gap between the separation kettle cylinder 41 and the spiral separator 43, flows out of the separation kettle through a gas outlet I413 arranged above the separation kettle cylinder 41, is filtered again through the filter 5, is refrigerated through a condenser and then is recycled into a CO2 storage tank 1 for the next use.
Example 2
8kg of flax roving bobbins are sequentially connected and sleeved in a bleaching kettle 3, H2O2The solution is a cosolvent and is placed in a cosolvent tank 8.
In the bleaching process, firstly, a refrigerating system is started, and liquid CO2Flows out of the CO2 storage tank 1 and is filtered by a filter 5 to remove impurities possibly contained. H in cosolvent tank 82O2The solution is injected into the CO-solvent inlet of the blender 2 by the liquid transfer pump 7, enters the pinhole transfer pipe inlet 26 through the CO-solvent channel 25, flows out of the pinhole transfer pipe outlet 27 through the pinhole transfer pipe 28, and is mixed with CO in the gas-liquid mixing channel 292And (4) fully mixing. CO2 dissolved with cosolvent uniformly is injected into the bleaching kettle 3 under the action of a high-pressure pump; and then enters a supercritical state under the action of the preheater 6.
Supercritical CO2Passing the fluid through CO2The gas-liquid mixture inlet 411 flows into the bleaching kettle 3, and flax cheese is output after being permeated and diffused from bottom to top; under the action of the magnetic circulation pump 11,CO2the fluid enters the bleaching kettle 3 again, the internal temperature of the bleaching kettle 3 is kept at 80 ℃, the pressure is 20MPa, and CO is kept2The flow rate of the fluid is 10g/min, and the bleaching circulation is realized for 60min by using the magnetic circulating pump 11 under the condition; the heat loss of the bleaching process is compensated by the heater 10.
After the bleaching process is completed, the magnetic circulation pump 11 is turned off. Supercritical CO in bleaching kettle 32The fluid enters a spiral tube type separator 43 in the multistage separation kettle 4, and under the action of the internal gradual change type filler, the fluid is kept at 3MPa and 20 ℃, so that the bleaching product and CO are mixed2Completely separating gas; and according to the molecular size, the extracted bleaching product is separated out via the spiral tube separator 43 and its filter sieve plate 434 in turn. The extract can be discharged through a liquid outlet 412 at the bottom of the separation vessel, and gaseous CO can be discharged2Then flows out through a gas outlet I413 at the upper end of the separation kettle. In the process, the bottom filter sieve plate 434 of the spiral tube separator 43 is located at the bottom of the separation vessel 4, thereby forming bottom-to-top CO2The gas gasification channel ensures the full gasification of gas. Gaseous CO2Flows out of the spiral tube separator 43, is filtered again by the filter 5, is refrigerated by the condenser and then is recycled into CO2Tank 1, for next use.
Passing through supercritical CO2After fluid bleaching, the whiteness of the flax roving is 61.5%, the weight loss rate is 9.3%, the residual gum rate is 10.9%, the breaking strength of a single fiber is 10.8cN/dtex, and the breaking elongation is 6.1%.
Example 3
5kg of flax roving bobbins are sequentially connected and sleeved in a bleaching kettle 3, H2O2The solution is a cosolvent and is placed in a cosolvent tank 8.
In the bleaching process, firstly, a refrigerating system is started, and liquid CO2In CO2The tank 1 is drained and filtered through a filter 5 to remove impurities that may be contained. H in cosolvent tank 82O2Solution in liquid transportThe CO-solvent is injected into the CO-solvent inlet of the blender 2 by the pump 7, enters the pinhole delivery pipe inlet 26 through the CO-solvent channel 25, flows out of the pinhole delivery pipe outlet 27 through the pinhole delivery pipe 28, and is fully mixed with CO2 in the gas-liquid mixing channel 29. CO2 dissolved with cosolvent uniformly is injected into the bleaching kettle 3 under the action of a high-pressure pump; and then enters a supercritical state under the action of the preheater 6.
Supercritical CO2Passing the fluid through CO2The gas-liquid mixture inlet 411 flows into the bleaching kettle 3, and flax cheese is output after being permeated and diffused from bottom to top; under the action of the magnetic circulating pump 11, CO2The fluid enters the bleaching kettle 3 again, the internal temperature of the bleaching kettle 3 is kept at 100 ℃, the pressure is 15MPa, and CO is kept2The flow rate of the fluid is 20g/min, and the bleaching circulation is realized for 90min by using the magnetic circulating pump 11 under the condition; the heat loss of the bleaching process is compensated by the heater 10.
After the bleaching process is completed, the magnetic circulation pump 11 is turned off. Supercritical CO in bleaching kettle 32The fluid enters a spiral tube type separator 43 in the multistage separation kettle 4, and under the action of the internal gradual change type filler, the fluid is kept at 3MPa and 20 ℃, so that the bleaching product and CO are mixed2Completely separating gas; and according to the molecular size, the extracted bleaching product is separated out via the spiral tube separator 43 and its filter sieve plate 434 in turn. The extract can be discharged through a liquid outlet 412 at the bottom of the separation vessel, and gaseous CO can be discharged2Then flows out through a gas outlet I413 at the upper end of the separation kettle. In the process, the bottom filter sieve plate 434 of the spiral tube separator 43 is located at the bottom of the separation vessel 4, thereby forming bottom-to-top CO2The gas gasification channel ensures the full gasification of gas. Gaseous CO2Flows out of the spiral tube separator 43, is filtered again by the filter 5, is refrigerated by the condenser and then is recycled into CO2Tank 1, for next use.
Passing through supercritical CO2After fluid bleaching, the whiteness of the flax roving is 58.5%, the weight loss rate is 8.1%, the residual gum rate is 11.3%, the breaking strength of a single fiber is 12.5cN/dtex, and the breaking elongation is 6.3%.
Example 4
Connecting and sleeving 10kg of flax roving bobbins in sequence into a bleaching kettle 3, and placing H2O2The solution is a cosolvent and is placed in a cosolvent tank 8.
In the bleaching process, firstly, a refrigerating system is started, and liquid CO2In CO2The tank 1 is drained and filtered through a filter 5 to remove impurities that may be contained. H in cosolvent tank 82O2The solution is injected into the CO-solvent inlet of blender 2 by liquid transfer pump 7, enters pinhole transfer tube inlet 26 through CO-solvent channel 25, exits pinhole transfer tube outlet 27 through pinhole transfer tube 28, and is thoroughly mixed with CO2 in gas-liquid mixing channel 29. CO2 dissolved with cosolvent uniformly is injected into the bleaching kettle 3 under the action of a high-pressure pump; and then enters a supercritical state under the action of the preheater 6.
Supercritical CO2Passing the fluid through CO2The gas-liquid mixture inlet 411 flows into the bleaching kettle 3, and flax cheese is output after being permeated and diffused from bottom to top; under the action of the magnetic circulating pump 11, CO2The fluid enters the bleaching kettle 3 again, the internal temperature of the bleaching kettle 3 is kept at 120 ℃, the pressure is 25MPa, and CO is kept2The flow rate of the fluid is 50g/min, and the bleaching circulation is realized for 60min by using the magnetic circulating pump 11 under the condition; the heat loss of the bleaching process is compensated by the heater 10.
After the bleaching process is completed, the magnetic circulation pump 11 is turned off. Supercritical CO in bleaching kettle 32The fluid enters a spiral tube type separator 43 in the multistage separation kettle 4, and under the action of the internal gradual change type filler, the fluid is kept at 3MPa and 20 ℃, so that the bleaching product and CO are mixed2Completely separating gas; and according to the molecular size, the extracted bleaching product is separated out via the spiral tube separator 43 and its filter sieve plate 434 in turn. The extract can be discharged through a liquid outlet 412 at the bottom of the separation vessel, and gaseous CO can be discharged2Then flows out through a gas outlet I413 at the upper end of the separation kettle. In the process, the bottom filter sieve plate 434 of the spiral tube separator 43 is located at the bottom of the separation vessel 4, thereby forming bottom-to-top CO2The gas gasification channel ensures the full gasification of gas. Gaseous CO2Flows out of the spiral tube separator 43, is filtered again by the filter 5, is refrigerated by the condenser and then is recycled into CO2Tank 1, for next use.
Passing through supercritical CO2After fluid bleaching, the whiteness of the flax roving is 61.8%, the weight loss rate is 8.8%, the residual gum rate is 11.5%, the breaking strength of a single fiber is 10.4cN/dtex, and the breaking elongation is 7.1%.
Example 5
Connecting and sleeving 15kg of flax roving bobbins in sequence into a bleaching kettle 3, and placing H2O2The solution is a cosolvent and is placed in a cosolvent tank 8.
In the bleaching process, firstly, a refrigerating system is started, and liquid CO2In CO2The tank 1 is drained and filtered through a filter 5 to remove impurities that may be contained. H in cosolvent tank 82O2The solution is injected into the CO-solvent inlet of the blender 2 by the liquid transfer pump 7, enters the pinhole transfer pipe inlet 26 through the CO-solvent channel 25, flows out of the pinhole transfer pipe outlet 27 through the pinhole transfer pipe 28, and is mixed with CO in the gas-liquid mixing channel 292And (4) fully mixing. CO2 dissolved with cosolvent uniformly is injected into the bleaching kettle 3 under the action of a high-pressure pump; and then enters a supercritical state under the action of the preheater 6.
Supercritical CO2Passing the fluid through CO2The gas-liquid mixture inlet 411 flows into the bleaching kettle 3, and flax cheese is output after being permeated and diffused from bottom to top; under the action of the magnetic circulating pump 11, CO2The fluid enters the bleaching kettle 3 again, the internal temperature of the bleaching kettle 3 is kept at 150 ℃, the pressure is 28MPa, and CO is kept2The flow rate of the fluid is 30g/min, and the bleaching circulation is realized for 150min by using the magnetic circulating pump 11 under the condition; heat loss of bleaching processLosses are compensated for by the heater 10.
After the bleaching process is completed, the magnetic circulation pump 11 is turned off. Supercritical CO in bleaching kettle 32The fluid enters a spiral tube type separator 43 in the multistage separation kettle 4, and under the action of the internal gradual change type filler, the fluid is kept at 3MPa and 20 ℃, so that the bleaching product and CO are mixed2Completely separating gas; and according to the molecular size, the extracted bleaching product is separated out via the spiral tube separator 43 and its filter sieve plate 434 in turn. The extract can be discharged through a liquid outlet 412 at the bottom of the separation vessel, and gaseous CO can be discharged2Then flows out through a gas outlet I413 at the upper end of the separation kettle. In the process, the bottom filter sieve plate 434 of the spiral tube separator 43 is located at the bottom of the separation vessel 4, thereby forming bottom-to-top CO2The gas gasification channel ensures the full gasification of gas. Gaseous CO2Flows out of the spiral tube separator 43, is filtered again by the filter 5, is refrigerated by the condenser and then is recycled into CO2Tank 1, for next use.
Passing through supercritical CO2After fluid bleaching, the whiteness of the flax roving is 65.6%, the weight loss rate is 9.2%, the residual gum rate is 10.5%, the breaking strength of a single fiber is 9.8cN/dtex, and the breaking elongation is 6.7%.
Example 6
Connecting and sleeving 12kg of flax roving bobbins in sequence into a bleaching kettle 3, and placing H2O2The solution is a cosolvent and is placed in a cosolvent tank 8.
In the bleaching process, firstly, a refrigerating system is started, and liquid CO2In CO2The tank 1 is drained and filtered through a filter 5 to remove impurities that may be contained. H in cosolvent tank 82O2The solution is injected into the CO-solvent inlet of blender 2 by liquid transfer pump 7, enters pinhole transfer tube inlet 26 through CO-solvent channel 25, exits pinhole transfer tube outlet 27 through pinhole transfer tube 28, and is thoroughly mixed with CO2 in gas-liquid mixing channel 29. Uniformly dissolvingCO2 dissolved with the cosolvent is injected into the bleaching kettle 3 under the action of a high-pressure pump; and then enters a supercritical state under the action of the preheater 6.
Supercritical CO2Passing the fluid through CO2The gas-liquid mixture inlet 411 flows into the bleaching kettle 3, and flax cheese is output after being permeated and diffused from bottom to top; under the action of the magnetic circulating pump 11, CO2The fluid enters the bleaching kettle 3 again, the internal temperature of the bleaching kettle 3 is kept at 130 ℃, the pressure is 25MPa, and CO is kept2The flow rate of the fluid is 40g/min, and the bleaching circulation is realized for 90min by using the magnetic circulating pump 11 under the condition; the heat loss of the bleaching process is compensated by the heater 10.
After the bleaching process is completed, the magnetic circulation pump 11 is turned off. Supercritical CO in bleaching kettle 32The fluid enters a spiral tube type separator 43 in the multistage separation kettle 4, and under the action of the internal gradual change type filler, the fluid is kept at 3MPa and 20 ℃, so that the bleaching product and CO are mixed2Completely separating gas; and according to the molecular size, the extracted bleaching product is separated out via the spiral tube separator 43 and its filter sieve plate 434 in turn. The extract can be discharged through a liquid outlet 412 at the bottom of the separation vessel, and gaseous CO can be discharged2Then flows out through a gas outlet I413 at the upper end of the separation kettle. In the process, the bottom filter sieve plate 434 of the spiral tube separator 43 is located at the bottom of the separation vessel 4, thereby forming bottom-to-top CO2The gas gasification channel ensures the full gasification of gas. Gaseous CO2Flows out of the spiral tube separator 43, is filtered again by the filter 5, is refrigerated by the condenser and then is recycled into CO2Tank 1, for next use.
Passing through supercritical CO2After fluid bleaching, the whiteness of the flax roving is 58.2%, the weight loss rate is 8.8%, the residual gum rate is 10.8%, the breaking strength of a single fiber is 9.1cN/dtex, and the breaking elongation is 5.4%.

Claims (9)

1. Supercritical CO of flax roving2An anhydrous bleaching plant comprising a structural unit CO2Storage tank, filter, blender, booster pump, preheater, heater, bleaching kettle, separation kettle, cosolvent tank, liquid delivery pump and magnetic circulation pump, wherein, CO2The storage tank, the filter, the blender, the booster pump, the preheater, the bleaching kettle and the separation kettle are sequentially connected through a pipeline, the cosolvent tank is connected with the blender after being connected with the liquid delivery pump through a pipeline, and the heater is communicated with the bleaching kettle upstream and downstream through a pipeline and used for enabling the bleaching kettle to be internally provided withHeating the materials; the magnetic circulating pump is communicated with the upstream and downstream of the bleaching kettle through a pipeline and is used for circulating materials in the bleaching kettle; it is characterized in that the preparation method is characterized in that,
the structural unit of the blender is as follows:
from CO2Inlet, CO2The outlet, the cosolvent inlet, the cosolvent passage, the pinhole conveying pipe inlet, the pinhole conveying pipe outlet, the pinhole conveying pipe and the gas-liquid mixing passage; the gas-liquid mixing channel is provided with a cavity with a cylindrical structure, a plurality of pinhole conveying pipes are uniformly distributed on the upper bottom surface and the lower bottom surface of the gas-liquid mixing channel respectively, the outer side end of each pinhole conveying pipe is communicated with the flat cylindrical cosolvent channel, and the center of the bottom surface of the cosolvent channel facing to the outer side is provided with a cosolvent inlet; CO is symmetrically arranged on the side wall of the cylindrical structure of the gas-liquid mixing channel2Inlet, CO2An outlet;
the separation kettle structure unit is as follows:
the gas-liquid mixer comprises a cylinder body and a top cover, wherein the cylinder body and the top cover are connected through a bolt, the cylinder body is provided with a gas-liquid mixture inlet, a liquid outlet and a gas outlet I, the gas-liquid mixture inlet is positioned on the side wall of the cylinder body, the liquid outlet is arranged below the cylinder body, and the gas outlet I is arranged above the cylinder body; fixedly connected with spiral separator in the barrel, spiral separator includes spiral pipe, spiral pipe entry end and spiral pipe exit end from top to bottom, the spiral pipe entry end is connected with the gas-liquid mixture entry, the spiral pipe exit end is connected with the liquid outlet, the sealed filter sieve that is provided with on the port inner wall of spiral pipe exit end, gas outlet II has been seted up on the spiral pipe exit end, gas outlet II is located filter sieve and spiral pipe between.
2. The bleaching apparatus according to claim 1, wherein the spiral tube is filled with a filler, the filler is silica gel or polystyrene, and the particle size of the filler is 1-10 μm.
3. The bleaching apparatus according to claim 2, wherein the particle size of the packing in the spiral tube decreases from the inlet of the gas-liquid mixture to the outlet II.
4. The bleaching apparatus according to claim 1 wherein the spiral separator is removably mounted within the barrel of the separation vessel.
5. The bleaching apparatus according to claim 1, wherein the separation vessel is at least one, and each separation vessel is connected in series by a pipeline.
6. The bleaching apparatus according to claim 1, wherein the pinhole ducts of the blender are arranged in the gas-liquid mixing passage in such a manner as to intersect at vertically opposite positions.
7. A bleaching method of flax roving, characterized in that the supercritical CO of flax roving as claimed in any one of claims 1-6 is adopted2The anhydrous bleaching device carries out bleaching.
8. The method of claim 7, wherein the method employs 30% H2O2The solution is a bleaching agent.
9. The method according to claim 8, wherein the bleaching conditions of the bleaching method are: supercritical CO2The fluid flow rate is 10-50g/min, the internal temperature of the bleaching kettle is 50-150 ℃, the pressure is 8-30MPa, and the bleaching time is 30-150 min.
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CN106676788B (en) * 2016-11-21 2019-01-08 大连工业大学 A kind of flax roving supercritical CO2Enzyme Scouring Process device and its kiering method
CN106835559B (en) * 2016-11-21 2019-01-08 大连工业大学 A kind of flax roving supercritical CO2Biobleaching device and its method for bleaching
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20050111982A (en) * 2004-05-24 2005-11-29 주식회사 삼일산업 Industrial supercritical fluid dye apparatus
CN1766194A (en) * 2005-11-17 2006-05-03 大连轻工业学院 Supercritical carbon dioxide dyeing device and its process
CN102787459A (en) * 2012-07-17 2012-11-21 大连工业大学 Supercritical carbon dioxide cheese dyeing kettle and waterless supercritical carbon dioxide cheese dyeing method
CN204734986U (en) * 2015-06-23 2015-11-04 江苏汉邦科技有限公司 Novel supercritical fluid chromatogram vapour and liquid separator
CN106676788A (en) * 2016-11-21 2017-05-17 大连工业大学 Flax thick yarn supercritical CO2 biological enzyme scouring device and scouring method thereof
CN106835559A (en) * 2016-11-21 2017-06-13 大连工业大学 A kind of flax roving supercritical CO2Biobleaching device and its method for bleaching

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20050111982A (en) * 2004-05-24 2005-11-29 주식회사 삼일산업 Industrial supercritical fluid dye apparatus
CN1766194A (en) * 2005-11-17 2006-05-03 大连轻工业学院 Supercritical carbon dioxide dyeing device and its process
CN102787459A (en) * 2012-07-17 2012-11-21 大连工业大学 Supercritical carbon dioxide cheese dyeing kettle and waterless supercritical carbon dioxide cheese dyeing method
CN204734986U (en) * 2015-06-23 2015-11-04 江苏汉邦科技有限公司 Novel supercritical fluid chromatogram vapour and liquid separator
CN106676788A (en) * 2016-11-21 2017-05-17 大连工业大学 Flax thick yarn supercritical CO2 biological enzyme scouring device and scouring method thereof
CN106835559A (en) * 2016-11-21 2017-06-13 大连工业大学 A kind of flax roving supercritical CO2Biobleaching device and its method for bleaching

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