CN218811780U - Natural VE of two-enzyme process draws preprocessing device - Google Patents
Natural VE of two-enzyme process draws preprocessing device Download PDFInfo
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- CN218811780U CN218811780U CN202123247418.7U CN202123247418U CN218811780U CN 218811780 U CN218811780 U CN 218811780U CN 202123247418 U CN202123247418 U CN 202123247418U CN 218811780 U CN218811780 U CN 218811780U
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Abstract
The utility model discloses a natural VE of double-enzyme process draws preprocessing device, including the enzyme retort, lipase recoverer, the crystallizer, the plate and frame filter, the transfer jar cauldron, first dehydration post, the blending tank, enzyme catalysis post and second dehydration post, the enzyme retort, lipase recoverer, first dehydration post, the blending tank, a plurality of is established respectively to enzyme catalysis post and second dehydration post, the enzyme retort is the same with the quantity of lipase recoverer and the one-to-one intercommunication, at least one lipase recoverer through corresponding the intercommunication communicates at least one crystallizer in proper order, the plate and frame filter, transfer jar cauldron, first dehydration post, the blending tank, enzyme catalysis post and second dehydration post entry, second dehydration post export and blending tank intercommunication. The utility model discloses a conversion rate that fatty acid methyl ester was improved to two steps of enzymatic process technologies realizes the used repeatedly of enzyme, and low cost reduces the production of acid-base waste water, reduces natural VE and draws the concentration degree of difficulty, environmental protection and energy saving.
Description
Technical Field
The utility model belongs to the technical field of biochemical industry, concretely relates to natural VE of two-enzyme process draws preprocessing device.
Background
The distillation method for extracting natural VE from deodorized distillate is a method commonly adopted at home and abroad. Under the condition of low oxygen and inertia, the distillation method has the advantages of low distillation temperature, short material heating time, high separation degree, no organic solvent residue and the like. The principle is that the difference of molecular motion free paths of different substances is used for realizing the separation of the substances, free fatty acid and glyceride in deodorized distillate are converted into fatty acid methyl ester with boiling point and molecular weight which are greatly different from those of natural VE, the fatty acid methyl ester is distilled out through distillation, and then the high-concentration natural VE is obtained through further concentration. The general process flow is shown in figure 1.
The methyl esterification process generally adopts concentrated sulfuric acid as a catalyst, and with the development of the biodiesel industry, a factory adopts a strong acid and strong base two-step catalysis method to improve the yield of fatty acid methyl ester. However, the use of a large amount of strong acid and strong base can generate a large amount of acid and alkali wastewater, and the difficulty of later separation and purification can be increased.
With the development of the biological enzyme technology, the enzymatic methyl esterification process is already applied to the biodiesel industry, but the enzymatic methyl esterification process is less applied to the natural VE extraction industry and is mainly limited by two factors: firstly, the conversion rate of fatty acid methyl ester in an enzymatic process is inferior to that of a chemical method, and the cost advantage is not great; secondly, in the existing factory, methyl esterification equipment is designed by a chemical method, the requirements of the existing enzymatic process cannot be met, and the equipment modification cost is high.
SUMMERY OF THE UTILITY MODEL
In order to solve the technical problem existing in the prior art, the utility model aims to provide a natural VE of two-enzyme method draws preprocessing device.
In order to realize the above purpose, reach above-mentioned technological effect, the utility model discloses a technical scheme be:
the utility model provides a natural VE of two enzyme methods draws preprocessing device, includes enzyme retort, lipase recoverer, crystallizer, plate and frame filter, transfer jar cauldron, first dehydration post, blending tank, enzyme catalysis post and second dehydration post, enzyme retort, lipase recoverer, first dehydration post, blending tank, enzyme catalysis post and second dehydration post are equipped with a plurality of respectively, and the first dehydration post of a plurality of communicates in proper order, and a plurality of enzyme catalysis post communicates in proper order, and a plurality of second dehydration post communicates in proper order, and the same and the one-to-one correspondence of quantity of enzyme retort and lipase recoverer communicates, and at least one enzyme retort communicates at least one crystallizer again in proper order through the lipase recoverer that corresponds the intercommunication and communicates plate and frame filter, jar transfer cauldron, first dehydration post, blending tank, enzyme catalysis post and second dehydration post entry, and second dehydration post export and blending tank intercommunication.
Furthermore, the number of the enzyme reaction tanks is two, namely a first enzyme reaction tank and a second enzyme reaction tank; the two lipase recoverers are respectively a first lipase recoverer and a second lipase recoverer; the two crystallization tanks are respectively a first crystallization tank and a second crystallization tank; the number of the first dehydration column, the number of the enzyme catalysis columns and the number of the second dehydration columns are two; the two mixing tanks are respectively a first mixing tank and a second mixing tank; the first enzyme reaction tank and the second enzyme reaction tank are arranged side by side and do not interfere with each other, the first enzyme reaction tank and the second enzyme reaction tank are respectively communicated with pipelines for introducing chilled water, hot water, methanol, deodorized distillate and water, the first enzyme reaction tank and the second enzyme reaction tank are both communicated with a first crystallizing tank and a second crystallizing tank, immobilized lipase in the first enzyme reaction tank and the second enzyme reaction tank is respectively recovered through a first lipase recoverer and a second lipase recoverer, the first crystallizing tank and the second crystallizing tank are both communicated with a plate frame filter and then sequentially communicated with a transfer tank kettle and a first dehydration column, the first dehydration column is respectively communicated with a first mixing tank and a second mixing tank, outlets of the first mixing tank and the second mixing tank are both communicated with an enzyme catalysis column through a fourth material pump and then communicated with an inlet of a second dehydration column, outlets of the second dehydration column are respectively communicated with inlets of the first mixing tank and the second mixing tank, and the first mixing tank are respectively communicated with pipelines for introducing hot water and methanol.
Furthermore, the first enzyme reaction tank and the second enzyme reaction tank are communicated with the first crystallizing tank and the second crystallizing tank through the first material pump.
Furthermore, the first crystallizing tank and the second crystallizing tank are communicated with the plate frame filter through a second material pump.
Furthermore, a third material pump is arranged between the transfer tank kettle and the first dehydration column.
Compared with the prior art, the beneficial effects of the utility model are that:
1. compared with the traditional enzyme method process, the utility model realizes the repeated use of the enzyme through the immobilized enzyme methyl esterification process, and reduces the cost of the enzyme method transesterification process;
2. the utility model improves the conversion rate of fatty acid methyl ester by a two-step enzyme method process, overcomes the defects of the existing enzyme method process, has stronger tolerance to methanol by the enzyme, and can add the methanol into a reaction container at one time, thereby simplifying the operation flow;
3. the double-enzyme method methyl esterification process is used for replacing the existing chemical methyl esterification process, the reaction conditions are milder, the recovery and the refining of the glycerol are facilitated, the generation of a large amount of acid-base wastewater is reduced, the difficulty in extracting and concentrating natural VE is reduced, the difficulty in refining the product is reduced, the operation is simple, and the advantages of environmental protection and energy conservation of the enzyme method process are exerted.
Drawings
FIG. 1 is a prior art process flow diagram;
FIG. 2 is a process flow diagram of the present invention;
fig. 3 is a schematic structural diagram of the present invention.
Detailed Description
The present invention is described in detail below to enable the advantages and features of the present invention to be more easily understood by those skilled in the art, thereby making more clear and definite definitions of the scope of the present invention.
The following presents a simplified summary of one or more aspects in order to provide a basic understanding of such aspects. This summary is not an extensive overview of all contemplated aspects, and is intended to neither identify key or critical elements of all aspects nor delineate the scope of any or all aspects. Its sole purpose is to present some concepts of one or more aspects in a simplified form as a prelude to the more detailed description that is presented later.
As shown in fig. 2-3, a dual-enzyme method natural VE extraction pretreatment device comprises a first enzyme reaction tank 1, a second enzyme reaction tank 2, a first lipase recoverer 3, a second lipase recoverer 4, a first material pump 5, a first crystallization tank 6, a second crystallization tank 7, a second material pump 8, a plate-and-frame filter 9, a transfer tank kettle 10, a third material pump 11, a first dehydration column 12, a first mixing tank 13, a second mixing tank 14, a fourth material pump 15, an enzyme catalysis column 16 and a second dehydration column 17, wherein the first enzyme reaction tank 1 and the second enzyme reaction tank 2 are the same, are arranged side by side and operate independently and do not interfere with each other, the first enzyme reaction tank 1 and the second enzyme reaction tank 2 are respectively communicated with pipelines for introducing chilled water, hot water, methanol, distillate and water, the first enzyme reaction tank 1 and the second enzyme reaction tank 2 are respectively communicated with a first crystallization tank 6 and a second crystallization tank 7 through the first material pump 5, the hot water, the methanol, the distillate and water in the first enzyme reaction tank 1 and the second enzyme reaction tank 2 are respectively communicated with the second crystallization tank 6 and the second crystallization tank 13 through the second mixing tank 13, the first material pump 14 and the second mixing tank 13 are respectively communicated with the second crystallization tank 13 inlets of the second mixing tank, the first enzyme reaction tank 13, the second mixing tank 13 is respectively communicated with the second mixing tank 14, the second mixing tank 13 and the second mixing tank 13 recycling tank 14, the second mixing tank 14 are respectively communicated with the inlets of the first enzyme reaction tank 13, the second mixing tank 13 mixing tank, the second mixing tank 13 recycling tank 14, the second mixing tank 14 and the second mixing tank 13 mixing tank 14, the second mixing tank 13 are respectively, and the recycling tank 13 mixing tank 14 are respectively communicated with the second mixing tank 13 mixing tank 14.
The double-enzyme method natural VE extraction pretreatment process comprises the following steps:
step one, carrying out methyl esterification reaction
The method comprises the steps of converting fatty acid and glyceride in deodorized distillate into fatty acid methyl ester under the catalysis of immobilized lipase under the condition of slightly excessive methanol, wherein the conversion can be carried out in an enzyme reaction tank or directly in an enamel reaction kettle by a chemical method by adopting an intermittent batch method; filtering, recovering immobilized lipase, putting into use again, separating sterol from the filtered matter by cold separation to obtain phytosterol, standing for separation, wherein the lower layer mainly comprises three substances of water, methanol and glycerol, recovering glycerol and methanol water solution at the lower layer, and performing step two on the unreacted free fatty acid in the upper oil phase;
step two, carrying out secondary methyl esterification reaction
The immobilized lipase is continuously used for catalyzing, a continuous reaction mode is adopted, the reaction is carried out towards the right side through physical dehydration, the acid value of a substrate is further reduced, the conversion rate of fatty acid methyl ester is improved, and the method specifically comprises the following steps:
separating to obtain an upper oil phase containing a part of free fatty acid, reacting incompletely, supplementing methanol, continuously catalyzing the free fatty acid and methanol methyl ester to be converted into fatty acid methyl ester by using immobilized lipase, removing generated water in a system to enable the reaction to move towards the right side, adopting a classical enzyme reaction column series structure, continuously reacting, then entering a natural VE distillation refining process, and sequentially distilling and molecular distilling to obtain VE.
In the first step, the mass of the methanol accounts for 16-20% of the total mass of the substrate, and the mass of the immobilized lipase accounts for 3-5% of the total mass of the substrate.
In the first step, the reaction temperature is 25-40 ℃, and the reaction time is 2-4h.
In the first step, the reaction mode is an enzyme reaction tank batch method mode.
The immobilized lipase used in the first step and the immobilized lipase used in the second step are both produced by Wuxi Youpuk Biotechnology GmbH, the lipase has strong tolerance to short-chain alcohol, the production cost is far lower than that of an imported immobilized enzyme preparation, and the lipase can catalyze both transesterification and ester synthesis.
In the step one, the methanol solution and the water-containing methanol recovered in the production process can be directly used in the enzyme method process in the step one without distillation and refining again.
In the second step, the mass of the supplemented methanol is 1-3% of the total mass of the substrate.
In the second step, the reaction temperature is 25-40 ℃.
A double-enzyme method natural VE extraction pretreatment device is adopted to carry out double-enzyme method natural VE extraction pretreatment, and the method specifically comprises the following steps:
1) Feeding the materials
Respectively injecting the deodorized distillate into a first enzyme reaction tank 1 and/or a second enzyme reaction tank 2, adjusting the pH value to 4.8-5.2 by using sodium hydroxide, adding methanol accounting for 16-20% of the total mass of the substrate and water accounting for 2% of the total mass of the substrate, starting stirring in the feeding process to uniformly mix, and introducing circulating water with the temperature of 25-40 ℃;
2) Enzyme reaction of
Adding immobilized lipase accounting for 3-5% of the total mass of the substrate into a corresponding enzyme reaction tank in the step 1), starting the reaction, maintaining stirring and stable temperature in the tank, finishing the reaction, and keeping the acid value of 4-8mg KOH/g and the reaction time of 2-4h;
3) And cold separation
Conveying the materials in the enzyme reaction tank in the step 2) to a first crystallization tank 6 and/or a second crystallization tank 7 through a first material pump 5, recovering the immobilized lipase in the first enzyme reaction tank 1 and the second enzyme reaction tank 2 through a first lipase recoverer 3 and a second lipase recoverer 4 respectively, and recycling the immobilized lipase, wherein the temperature of the materials in the first crystallization tank 6 and/or the second crystallization tank 7 is reduced to below 10 ℃, and recovering the separated sterol through a plate and frame filter 9;
4) And settling of the mixture
Collecting filtrate filtered by a plate and frame filter 9 in a transfer pot kettle 10, standing and separating out lower-layer glycerol methanol solution, conveying upper-layer oil phase by a third material pump 11, dehydrating by a first dehydration column 12, and then entering a first mixing tank 13 and/or a second mixing tank 14;
5) And then methyl esterification is carried out again
In the methyl ester esterification again, the immobilized lipase is used for continuously catalyzing the reaction of the incompletely reacted free fatty acid and methanol, the methanol accounting for 1 to 3 percent of the total mass of the substrate is supplemented in the first mixing tank 13 and/or the second mixing tank 14, the stirring is started, and the circulating water with the temperature of 25 to 40 ℃ is introduced. The material is circularly conveyed by a fourth material pump 15, sequentially passes through an enzyme catalysis column 16 and a second dehydration column 17, then enters a first mixing tank 13 and/or a second mixing tank 14, and is dehydrated before and after the substrate is reacted by the second dehydration column 17, so that the reaction is carried out towards the right side. When the acid value of the substrate is reduced to 1.8-2.5mgKOH/g, the material can enter a refining link.
It should be noted that the enzyme catalysis column 16 and the second dehydration column 17 are connected in series in multiple sets, and can be replaced in the production process. The hydrous methanol generated in the production process can be directly used for the methyl esterification reaction in the step one, and dehydration and refining are not needed.
The first enzyme reaction tank 1, the second enzyme reaction tank 2, the first crystallizing tank 6, the second crystallizing tank 7, the transfer tank kettle 10, the first mixing tank 13, the second mixing tank 14 and the like can adjust the number and size of equipment according to specific productivity and production requirements, so that the production is smoother.
Example 1
The deodorized distillate is mainly prepared from soybean oil and rapeseed oil, but is not limited to the deodorized distillate prepared from oil crops.
Accurately weighing 200g of soybean deodorized distillate (acid value is 96.15 mgKOH/g), adding 32g of methanol and 4g of water, stirring uniformly, heating a substrate to 30 ℃, adding 6g of immobilized lipase, reacting for 4 hours, wherein the acid value is 4.62mgKOH/g after the reaction is finished, filtering and recovering the immobilized lipase, reducing the temperature of the material to 8 ℃, and performing suction filtration and recovery of sterol by using 200-mesh gauze; standing, separating, recovering lower layer glycerol and methanol water solution, repeating the above steps with recovered immobilized lipase, continuously using 20 batches, wherein the batch with the highest acid value is 6.24mgKOH/g, and the activity of the immobilized lipase is not significantly reduced;
and collecting the 20 batches of reaction substrates, adding 2g of methanol, uniformly mixing, and measuring the acid value to be 5.46mgKOH/g. Dehydrating the material, carrying out esterification reaction again by using an enzyme reaction column, finally reducing the acid value of the material to 2.44mgKOH/g, and entering a refining link.
Example 2
The deodorized distillate is mainly prepared from soybean oil and rapeseed oil, but is not limited to the deodorized distillate prepared from oil crops.
Accurately weighing 200g of soybean deodorized distillate (acid value is 96.15 mgKOH/g), adding 35g of methanol and 4g of water, stirring uniformly, heating a substrate to 30 ℃, adding 8g of immobilized lipase, reacting for 3 hours, filtering and recovering the immobilized lipase, reducing the temperature of the material to 8 ℃, and performing suction filtration by using 200-mesh gauze to recover sterol, wherein the acid value is less than 7mgKOH/g after the reaction is finished; standing, separating, recovering lower layer glycerol and methanol water solution, repeating the above steps with recovered immobilized lipase, continuously using 20 batches, wherein the batch with the highest acid value is not more than 7mgKOH/g, and the activity of the immobilized lipase is not remarkably reduced;
and (3) collecting the reaction substrates of the 20 batches, adding 4g of methanol, uniformly mixing, dehydrating the materials, carrying out esterification reaction again by using an enzyme reaction column, and finally, entering a refining link after the acid value of the materials is reduced to be below 2.5 mgKOH/g.
The same as in example 1.
Example 3
The deodorized distillate is mainly the byproducts of soybean oil and rapeseed oil processing, but is not limited to the deodorized distillate of oil crop processing.
Accurately weighing 200g of soybean deodorized distillate (acid value 96.15 mgKOH/g), injecting into a first enzyme reaction tank 1, adjusting pH to about 5 with sodium hydroxide, adding 40g of methanol and 4g of water, stirring during the charging process to mix uniformly, and introducing circulating water at 25 ℃; heating a substrate to 25 ℃, adding 10g of immobilized lipase, reacting for 4 hours, wherein the acid value is 4-8mgKOH/g after the reaction is finished, conveying the material in a first enzyme reaction tank 1 to a first crystallization tank 6 through a first material pump 5, recovering the immobilized lipase in the first enzyme reaction tank 1 through a first lipase recoverer 3, recycling the immobilized lipase, reducing the temperature of the material in the first crystallization tank 6 to below 10 ℃, and recovering the separated sterol through a plate and frame filter 9; and collecting filtrate filtered by a plate and frame filter 9 in a transfer tank kettle 10, standing to separate a lower layer of glycerol and methanol aqueous solution, conveying an upper layer of oil phase by a third material pump 11, dehydrating by a first dehydration column 12, then feeding the dehydrated upper layer of oil phase into a first mixing tank 13, adding 6g of methanol, mixing uniformly, dehydrating the material, carrying out esterification reaction again by using an enzyme reaction column, and finally feeding the dehydrated upper layer of oil phase into a refining link after the acid value of the material is reduced to be below 2.5 mgKOH/g.
The same as in example 1.
The utility model discloses the part or the structure that do not specifically describe adopt prior art or current product can, do not do here and describe repeatedly.
The above only is the embodiment of the present invention, not limiting the patent scope of the present invention, all utilize the equivalent structure or equivalent flow transformation that the content of the specification does, or directly or indirectly use in other related technical fields, all including in the same way the patent protection scope of the present invention.
Claims (4)
1. A natural VE extraction pretreatment device adopting a double-enzyme method is characterized by comprising an enzyme reaction tank, a lipase recoverer, a crystallization tank, a plate frame filter, a transfer tank kettle, a first dehydration column, a mixing tank, an enzyme catalysis column and a second dehydration column, wherein the enzyme reaction tank, the lipase recoverer, the first dehydration column, the mixing tank, the enzyme catalysis column and the second dehydration column are respectively provided with a plurality of devices, the first dehydration columns are sequentially communicated, the enzyme catalysis columns are sequentially communicated, the second dehydration columns are sequentially communicated, the enzyme reaction tank and the lipase recoverer are same in number and are communicated in a one-to-one correspondence manner, at least one enzyme reaction tank is communicated with at least one crystallization tank through the corresponding communicated lipase recoverer and then is sequentially communicated with the plate frame filter, the transfer tank kettle, the first dehydration column, the mixing tank, the enzyme catalysis column and an inlet of the second dehydration column, and an outlet of the second dehydration column is communicated with the mixing tank;
the two enzyme reaction tanks are respectively a first enzyme reaction tank and a second enzyme reaction tank; the two lipase recoverers are respectively a first lipase recoverer and a second lipase recoverer; the two crystallization tanks are respectively a first crystallization tank and a second crystallization tank; the number of the first dehydration column, the number of the enzyme catalysis column and the number of the second dehydration column are two; the two mixing tanks are respectively a first mixing tank and a second mixing tank; the first enzyme reaction tank and the second enzyme reaction tank are arranged side by side and do not interfere with each other, the first enzyme reaction tank and the second enzyme reaction tank are respectively communicated with pipelines for introducing chilled water, hot water, methanol, deodorized distillate and water, the first enzyme reaction tank and the second enzyme reaction tank are both communicated with a first crystallizing tank and a second crystallizing tank, immobilized lipase in the first enzyme reaction tank and the second enzyme reaction tank is respectively recovered through a first lipase recoverer and a second lipase recoverer, the first crystallizing tank and the second crystallizing tank are both communicated with a plate frame filter and then sequentially communicated with a transfer tank kettle and a first dehydration column, the first dehydration column is respectively communicated with a first mixing tank and a second mixing tank, outlets of the first mixing tank and the second mixing tank are both communicated with an enzyme catalysis column through a fourth material pump and then communicated with an inlet of a second dehydration column, outlets of the second dehydration column are respectively communicated with inlets of the first mixing tank and the second mixing tank, and the first mixing tank are respectively communicated with pipelines for introducing hot water and methanol.
2. The dual-enzyme method natural VE extraction pretreatment device according to claim 1, wherein the first enzyme reaction tank and the second enzyme reaction tank are communicated with the first crystallization tank and the second crystallization tank through a first material pump.
3. The dual-enzyme method natural VE extraction pretreatment device of claim 1, wherein the first crystallization tank and the second crystallization tank are both communicated with a plate and frame filter through a second material pump.
4. The pretreatment device for extracting VE by a two-enzyme method according to claim 1, wherein a third material pump is arranged between the middle-conversion tank kettle and the first dehydration column.
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| CN202123247418.7U CN218811780U (en) | 2021-12-22 | 2021-12-22 | Natural VE of two-enzyme process draws preprocessing device |
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| CN202123247418.7U CN218811780U (en) | 2021-12-22 | 2021-12-22 | Natural VE of two-enzyme process draws preprocessing device |
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