CN107583308B - Equipment and process for purifying 1, 3-propylene glycol and 2, 3-butanediol - Google Patents
Equipment and process for purifying 1, 3-propylene glycol and 2, 3-butanediol Download PDFInfo
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Abstract
The invention provides equipment and a process for purifying 1, 3-propylene glycol and 2, 3-butanediol, which comprise a granular carbon adsorption tank (10) with a material inlet (5), an air inlet (6), an air outlet (7), a water outlet (8), a silk screen (11), a filtering sieve plate (14), quartz sand (13), a carbon discharge port (12), a sight glass (9) and a backwash water inlet (16) and a matched part, wherein one end of a feed pump (2A) of the matched part is connected with a raw material tank (1A), the other end of the feed pump is connected with a regulating valve (3), the opening of the regulating valve is controlled through a flowmeter (4), the flowmeter (4) is connected with the material inlet (5) of the granular carbon adsorption tank, the carbon discharge port (12) of the granular carbon adsorption tank is connected with a granular carbon separation tank (15), the granular carbon separation tank is connected with a water pump (2B), and the other end of the safety filter is connected with a product tank (1B) and a disqualified product tank (1C). The adsorption tank disclosed by the invention has a simple structure, is convenient to operate and clean to wash, can reduce the chromaticity and ultraviolet absorbance of a product, improves the quality of the product, and meets the requirements of a polymerization grade product.
Description
Technical Field
The invention belongs to the field of biochemical engineering, and in particular relates to equipment and a process for purifying 1, 3-propanediol and 2, 3-butanediol produced by a fermentation method.
Background
1, 3-Propanediol (PDO) and 2, 3-Butanediol (BDO) are important chemical raw materials, and PDO is a key raw material for synthesizing the memory fiber polytrimethylene terephthalate (PTT). Biological PDO production technology has long been monopolized by dupont, making PTT fibers difficult to mass produce. The company and the university of Qinghua cooperate to develop the PDO production technology and implement the industrial production of the bio-based PDO technology so as to meet the requirements of PTT polymerization factories.
BDO can be directly used in various industries as a chemical product, for example, can be used as an organic solvent, a cosmetic raw material, a flavor additive, an additive of fuel and the like.
In the process of producing PDO and BDO by a microbial fermentation method, fermentation liquor is light yellow due to the fact that pigment is contained, the application of the PDO and BDO of the product is affected by the existence of the pigment, and therefore, in order to obtain qualified PDO and BDO, the product must be subjected to decolorization treatment. The conventional decolorizing process includes decolorizing with active carbon, and Liu Dehua, and is one kind of decolorizing treatment of PDO rectifying product with active carbon column or macroporous resin column (Liu Dehua. Purifying 1, 3-propylene glycol from 1, 3-propylene glycol fermenting liquid and its application [ P ]. Chinese patent No. 201510206096.1.2015-07-22).
At present, the decolorization is mainly divided into two types of intermittent decolorization of powdered carbon and continuous decolorization of granular carbon, and compared with the intermittent decolorization of the powdered carbon, the continuous decolorization of the granular carbon has the characteristics of low labor intensity, simple and convenient operation, high product quality and the like. At present, an adsorption tower for continuously decoloring granular carbon has various forms, cao of Tianjin Laiyi technologies Co., ltd.develops an activated carbon decoloring refining tower (Cao. An activated carbon adsorbing decoloring refining tower [ P ]. Chinese patent: 201220538018.3.2012-10-19), yan Zeqin of Chengdu Shanghuang biological technologies Co., ltd.develops a decoloring tank (Yan Zeqin. Decoloring tank [ P ]. Chinese patent: 201420044392.7.2014-01-24), ni Zhen of Sanyo Rui oil processing Co., ltd.) develops an industrial glycerin decoloring device (Ni Zhen. An industrial glycerin decoloring device [ P ]. Chinese patent: 201520344427.3.2015-05-26). These patents suffer from the following disadvantages: 1) The carbon loading and the carbon discharging are inconvenient; 2) The design of the components of the decoloring tank is too simple, and the processes of back flushing, air exhaust and the like before the use of the activated carbon cannot be realized.
In addition, ultraviolet absorbance is an important index reflecting the quality of a PDO product, and the ultraviolet absorbance of the PDO affects important parameters of the product in the application of synthesizing a high polymer, so that the ultraviolet absorbance of the PDO product is difficult to be reduced to below 0.1 (270 nm) in the prior art, and the application of the PDO product in polymerization is affected.
Disclosure of Invention
The invention aims to make up the defects in the prior art, and provides equipment and a process for purifying 1, 3-propanediol and 2, 3-butanediol, which can reduce the chromaticity and ultraviolet absorbance of products, improve the quality of the products and meet the requirements of polymer grade products.
In order to achieve the aim, the equipment for purifying the 1, 3-propylene glycol and the 2, 3-butanediol is characterized by comprising a core component granular carbon adsorption tank and matched components, wherein the granular carbon adsorption tank is provided with a material inlet, an air outlet, a water outlet, a silk screen, a filtering screen plate, quartz sand, a carbon discharge port, a sight glass and a backwash water inlet, wherein the material inlet, the air inlet and the air outlet are positioned on an upper end enclosure of the adsorption tank, the water outlet is positioned on the side surface of the upper part of the adsorption tank body, the sight glass is arranged on the front surface of the upper part of the adsorption tank body, the lower end enclosure is provided with a backwash water inlet, the silk screen, quartz sand and the filtering screen plate are positioned on the lower part of the adsorption tank, the quartz sand is positioned between the silk screen and the filtering screen plate, and the carbon discharge port is positioned on the side surface of the lower part of the adsorption tank body; the supporting parts of adsorption tank have head tank, charge pump, governing valve, flowmeter, particle carbon separation jar, water pump, cartridge filter, product jar, disqualification product jar, wherein head tank is connected to charge pump one end, and the governing valve is connected to one end to through the aperture of flowmeter control governing valve, the material entry of particle carbon adsorption jar is connected to the flowmeter, particle carbon separation jar is connected to the row charcoal mouth of particle carbon adsorption jar, particle carbon separation jar is connected with the water pump, cartridge filter is connected with particle carbon adsorption jar, cartridge filter's the other end is connected product jar and disqualification product jar.
In the technical scheme, the feeding flow is controlled by the flow meter and the regulating valve in a linkage way, the flow meter has a signal feedback function, after a certain flow is set, the flow meter outputs a feedback signal to the regulating valve, and the opening of the regulating valve changes after receiving the feedback signal of the flow meter until the reading of the flow meter is consistent with the set flow;
in the technical scheme, the water outlet and the backflushing water inlet of the adsorption tank are used for flushing granular carbon, after the granular carbon is filled into the tank, the backflushing water is fed from the backflushing water inlet of the tank bottom to backflush the granular carbon, so that the powdery carbon in the granular carbon is cleaned, and water and the powdery carbon are discharged from the water outlet at the upper side surface of the cylinder body of the adsorption tank;
in the technical scheme, the exhaust port is used for exhausting air in the granular carbon, the granular carbon is developed in gaps, a large amount of air is arranged in the pores after cleaning and draining, and after feeding, the air in the pores is continuously exhausted through the exhaust port;
in the technical scheme, the carbon discharging port is used for discharging granular carbon, under the condition that water is filled in the granular carbon adsorption tank, the granular carbon can smoothly flow out of the tank, the flowing granular carbon and water are separated through the granular carbon separation tank, the separated granular carbon is packaged, and the water is pumped back to the adsorption tank through the water pump for repeated use;
in the technical scheme, the granular carbon adsorption tank consists of 1 or more adsorption tanks which are connected in series, so that the adsorption performance of granular carbon is fully exerted, and the granular carbon in any one adsorption tank is disconnected from equipment after being adsorbed and saturated, so that the granular carbon can be conveniently replaced;
in the technical scheme, the cartridge filter is used for filtering the decolorized solution, the filter medium is a titanium metal, ceramic or organic film, and the pore diameter of the filter medium is 0.5-5 mu m.
The equipment can adsorb and remove pigments and impurities in PDO and BDO materials, rinse and recycle the PDO and BDO materials adsorbed by the granular carbon, and smoothly discharge the adsorbed and saturated granular carbon from the adsorption tank. After the granular carbon is saturated to the PDO or BDO materials, the waste carbon is used for rinsing the PDO or BDO materials, the granular carbon soaked in the water can be smoothly discharged to the granular carbon separating tank from the carbon discharging port together with the water, the granular carbon and the water are subjected to solid-liquid separation in the separating tank, the water permeates the filter plate in the separating tank, the granular carbon is trapped by the filter plate, a certain included angle is formed between the filter plate and the horizontal direction, and the granular carbon is pushed out from the outlet on the side face of the separating tank and is filled into the packaging bag.
A process for the purification of 1, 3-propanediol and 2, 3-butanediol comprising the steps of:
1) After the granular carbon is filled into the adsorption tank, the granular carbon is backwashed by water inlet from a backwater water inlet at the bottom of the adsorption tank, and the powdery carbon and ash are discharged from a water outlet;
2) After PDO or BDO materials enter the adsorption tank, air in the granular carbon is discharged through the exhaust port;
3) After the exhaust is completed, after PDO or BDO materials flow out of the exhaust port, the exhaust port is closed, the opening of an outlet valve at the bottom of the adsorption tank is adjusted, and the materials are adsorbed and decolored through a silk screen, quartz sand and a filtering sieve plate;
4) The PDO or BDO material after decolorization and adsorption enters an unqualified product tank after passing through a cartridge filter due to high water content, and enters a qualified product tank after water is qualified;
5) After the granular carbon is adsorbed and saturated, compressed air is introduced through an air inlet to blow the PDO or BDO materials in the adsorption tank as much as possible, water is introduced from a material inlet at the top of the adsorption tank for rinsing, PDO or BDO materials in the adsorption tank are recovered, and rinsing water enters an unqualified product tank;
6) After the rinsing is finished, a certain amount of water is kept in the adsorption tank, a carbon discharge port is opened, so that the water and the granular carbon are discharged and flow into the granular carbon separation tank, after separation, the granular carbon is filled into a packaging bag, and after the water passes through a filter plate in the granular carbon separation tank, the water is pumped back into the adsorption tank by a water pump for repeated use.
The beneficial effects of the invention are as follows:
1) The granular carbon adsorption tank has a simple structure, smooth carbon discharge and convenient bagging after the granular carbon saturated in adsorption is discharged through the granular carbon separation tank;
2) The granular carbon adsorption tank is provided with a bottom backwash water inlet and an upper water outlet, so that powder carbon and ash in the granular carbon can be conveniently and rapidly washed clean;
3) The granular carbon adsorption tanks are connected in series by 1 or more, can fully exert the adsorption performance of granular carbon, and can be disconnected from the equipment after the granular carbon in any one adsorption tank is saturated for convenient replacement of granular carbon,
4) The chromaticity and absorbance of the PDO product are obviously reduced, and the quality of the product is greatly improved.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Wherein: 1A, a raw material tank; 2A is a feed pump; 2B is a water pump; 3 is a regulating valve; 4 is a flow meter; 5 is a material inlet; 6 is an air inlet; 7 is an exhaust port; 8 is a water outlet; 9 is a sight glass; 10 is a granular carbon canister; 11 is a wire mesh; 12 is a carbon discharging port; 13 is quartz sand; 14 is a filter screen panel; 15 is a granular carbon separator tank; 16 is a backwash water inlet; 17 is a cartridge filter; 1B a product tank; 1C is a reject pot.
Detailed Description
The present invention will be described in detail with reference to examples.
The invention discloses equipment for purifying 1, 3-propylene glycol and 2, 3-butanediol, which comprises a granular carbon adsorption tank (10) with a material inlet (5), an air inlet (6), an air outlet (7), a water outlet (8), a silk screen (11), a filtering sieve plate (14), quartz sand (13), a carbon outlet (12), a sight glass (9) and a backwash water inlet (16) and a matching component, wherein one end of a feed pump (2A) of the matching component is connected with a raw material tank (1A), the other end of the feed pump is connected with a regulating valve (3), the opening of the regulating valve is controlled through a flowmeter (4), the flowmeter (4) is connected with the material inlet (5) of the granular carbon adsorption tank, the carbon outlet (12) of the granular carbon adsorption tank is connected with a granular carbon separation tank (15), the granular carbon separation tank is connected with a water pump (2B), a security filter (17) is connected with the granular carbon adsorption tank, and the other end of the security filter is connected with a product tank (1B) and a disqualified product tank (1C). The utility model provides a granule charcoal adsorption tank, material entry (5), air inlet (6), gas vent (7) are located the adsorption tank upper end enclosure, outlet (8) are located adsorption tank barrel upper portion side, sight glass (9) are installed in the front on adsorption tank barrel upper portion, the low head has backwash water entry (16), silk screen (11), quartz sand (13), filter screen (14) are located the lower part in the adsorption tank, quartz sand is between silk screen and filter screen, carbon discharge mouth (12) are located adsorption tank barrel lower part side.
The operation steps of the device are as follows:
1) After the granular carbon is filled into the adsorption tank, water is fed from a backwash water inlet (16) at the bottom of the adsorption tank to backwash the granular carbon, and powder carbon and ash are discharged from a water outlet (8);
2) After PDO or BDO materials enter the adsorption tank, air in the granular carbon is discharged through an exhaust port (7);
3) After the exhaust is completed, after PDO or BDO materials flow out of the exhaust port (7), the exhaust port (7) is closed, the opening of an outlet valve at the bottom of the adsorption tank is adjusted, and the materials are adsorbed and decolored through a silk screen (11), quartz sand (13) and a filtering screen plate (14);
4) The PDO or BDO material after decolorization and adsorption enters an unqualified product tank (1C) after passing through a cartridge filter (17) due to high water content, and enters a qualified product tank (1B) after the water content is qualified;
5) After the granular carbon is adsorbed and saturated, compressed air is fed through an air inlet (6) to blow the PDO or BDO materials in the adsorption tank to the greatest extent, water is fed into the adsorption tank from a material inlet (5) at the top of the adsorption tank for rinsing, the PDO or BDO materials in the adsorption tank are recovered, and the rinsing water is fed into a non-conforming product tank (1C);
6) After the rinsing is finished, a certain amount of water is kept in the adsorption tank, a carbon discharge port (12) is opened, so that the water and the granular carbon are discharged and flow into a granular carbon separation tank (15), after separation, the granular carbon is filled into a packaging bag, and after the water passes through a filter plate in the granular carbon separation tank, the water is pumped back into the adsorption tank by a water pump (2B) for repeated use.
The PDO and BDO feedstocks were adsorbed by this process and the parameters before and after the adsorption treatment are shown in the following table.
TABLE 1 comparison of index before and after adsorption of PDO and BDO raw materials by granular carbon
According to the equipment and the process, the granular carbon adsorption tank is simple in structure, smooth in carbon discharge, and convenient to pack after the granular carbon subjected to adsorption saturation is discharged through the granular carbon separation tank; the granular carbon adsorption tank is provided with a bottom backwash water inlet and an upper water outlet, so that powder carbon and ash in the granular carbon can be conveniently and rapidly washed clean; the granular carbon adsorption tanks are connected in series by 1 or more, so that the adsorption performance of the granular carbon can be fully exerted, wherein after the granular carbon in any one adsorption tank is saturated in adsorption, the adsorption tank is disconnected from the equipment, and the granular carbon can be conveniently replaced; the chromaticity and absorbance of the PDO product are obviously reduced, and the quality of the product is greatly improved.
Of course, the above description is not intended to limit the invention, but rather the invention is not limited to the above examples, and variations, modifications, additions or substitutions within the spirit and scope of the invention will be within the scope of the invention.
Claims (1)
1. A process for purifying 1, 3-propanediol or 2, 3-butanediol, characterized in that the process employs a purification apparatus comprising:
the particle carbon adsorption tank is provided with a material inlet, an air outlet, a water outlet, a silk screen, a filtering sieve plate, quartz sand, a carbon discharge port, a sight glass and a backwash water inlet, wherein the material inlet, the air inlet and the air outlet are positioned on the upper end socket of the particle carbon adsorption tank, the water outlet is positioned on the side surface of the upper part of the particle carbon adsorption tank, the sight glass is arranged on the front surface of the upper part of the particle carbon adsorption tank, the backwash water inlet is arranged on the lower end socket of the particle carbon adsorption tank, the silk screen, the quartz sand and the filtering sieve plate are positioned on the lower part of the particle carbon adsorption tank, the quartz sand is positioned between the silk screen and the filtering sieve plate, and the carbon discharge port is positioned on the side surface of the lower part of the particle carbon adsorption tank; the auxiliary components of the adsorption tank comprise a raw material tank, a feed pump, a regulating valve, a flowmeter, a granular carbon separation tank, a water pump, a security filter, a product tank and an unqualified product tank, wherein one end of the feed pump is connected with the raw material tank, the other end of the feed pump is connected with the regulating valve, the opening of the regulating valve is controlled through the flowmeter, the flowmeter is connected with a material inlet of the granular carbon adsorption tank, a carbon discharge port of the granular carbon adsorption tank is connected with the granular carbon separation tank, the granular carbon separation tank is connected with the water pump, the security filter is connected with the granular carbon adsorption tank, and the other end of the security filter is connected with the product tank and the unqualified product tank;
the filtering sieve plate has a certain included angle with the horizontal direction, and granular carbon is discharged from a carbon discharge port on the side surface of the granular carbon adsorption tank;
the filter medium of the cartridge filter is titanium metal, ceramic or organic film, and the aperture of the filter medium is 0.5-5 mu m;
the granular carbon adsorption tanks are connected in series, and when any granular carbon adsorption tank is saturated in adsorption, the granular carbon adsorption tank is disconnected from the equipment;
the process comprises the following steps:
1) After the granular carbon is filled into the granular carbon adsorption tank, water is fed from a backwash water inlet at the bottom of the granular carbon adsorption tank to backwash the granular carbon, and powder carbon and ash are discharged from a water outlet;
2) After the 1, 3-propanediol or 2, 3-butanediol material enters the granular carbon adsorption tank, the air in the granular carbon is discharged through the exhaust port;
3) After the exhaust is completed, the exhaust port is closed after the 1, 3-propanediol or 2, 3-butanediol material flows out, the opening of an outlet valve at the bottom of the granular carbon adsorption tank is regulated, and the material adsorption decolorization operation is carried out through a silk screen, quartz sand and a filtering sieve plate;
4) The decolored and adsorbed 1, 3-propanediol or 2, 3-butanediol material is fed into an unqualified product tank after passing through a security filter due to high water content, and fed into a qualified product tank after water is qualified;
5) After the granular carbon is adsorbed and saturated, compressed air is introduced through an air inlet to blow the 1, 3-propanediol or 2, 3-butanediol material in the adsorption tank as much as possible, water is introduced into the adsorption tank from a material inlet at the top of the granular carbon adsorption tank for rinsing, the 1, 3-propanediol or 2, 3-butanediol material in the adsorption tank is recovered, and rinsing water is introduced into a non-qualified product tank;
6) After the rinsing is finished, a certain amount of water is kept in the granular carbon adsorption tank, a carbon discharge port is opened to discharge water and granular carbon, the water and the granular carbon flow into the granular carbon separation tank, after separation, the granular carbon is filled into a packaging bag, and after the water passes through a filter plate in the granular carbon separation tank, the water is pumped back into the granular carbon adsorption tank by a water pump for repeated use.
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