CN111909391A - Industrial production process and equipment for eucommia ulmoides rubber - Google Patents
Industrial production process and equipment for eucommia ulmoides rubber Download PDFInfo
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- CN111909391A CN111909391A CN202010897320.7A CN202010897320A CN111909391A CN 111909391 A CN111909391 A CN 111909391A CN 202010897320 A CN202010897320 A CN 202010897320A CN 111909391 A CN111909391 A CN 111909391A
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 55
- 241000208689 Eucommia ulmoides Species 0.000 title claims abstract description 50
- 238000009776 industrial production Methods 0.000 title claims abstract description 21
- 239000003292 glue Substances 0.000 claims abstract description 118
- 241000208688 Eucommia Species 0.000 claims abstract description 46
- 239000002904 solvent Substances 0.000 claims abstract description 35
- 238000001035 drying Methods 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 27
- 239000000899 Gutta-Percha Substances 0.000 claims abstract description 15
- 240000000342 Palaquium gutta Species 0.000 claims abstract description 15
- 229920000588 gutta-percha Polymers 0.000 claims abstract description 15
- 230000001112 coagulating effect Effects 0.000 claims abstract description 8
- 238000000638 solvent extraction Methods 0.000 claims abstract description 3
- 238000000605 extraction Methods 0.000 claims description 65
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 28
- 238000009833 condensation Methods 0.000 claims description 25
- 230000005494 condensation Effects 0.000 claims description 25
- 239000010903 husk Substances 0.000 claims description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 17
- 239000002994 raw material Substances 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 15
- 239000003208 petroleum Substances 0.000 claims description 14
- 238000000926 separation method Methods 0.000 claims description 14
- 238000005345 coagulation Methods 0.000 claims description 12
- 230000015271 coagulation Effects 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- 102000004190 Enzymes Human genes 0.000 claims description 11
- 108090000790 Enzymes Proteins 0.000 claims description 11
- 229940088598 enzyme Drugs 0.000 claims description 11
- 108010059892 Cellulase Proteins 0.000 claims description 10
- 108010059820 Polygalacturonase Proteins 0.000 claims description 10
- 229940106157 cellulase Drugs 0.000 claims description 10
- 108010093305 exopolygalacturonase Proteins 0.000 claims description 10
- 239000003960 organic solvent Substances 0.000 claims description 10
- 108091005508 Acid proteases Proteins 0.000 claims description 9
- 230000008014 freezing Effects 0.000 claims description 9
- 238000007710 freezing Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 239000003223 protective agent Substances 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000004062 sedimentation Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 230000000415 inactivating effect Effects 0.000 claims description 7
- 239000004568 cement Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 238000010092 rubber production Methods 0.000 abstract description 2
- 239000008394 flocculating agent Substances 0.000 description 8
- 238000003756 stirring Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 5
- 238000005189 flocculation Methods 0.000 description 4
- 230000016615 flocculation Effects 0.000 description 4
- 239000004816 latex Substances 0.000 description 4
- 229920000126 latex Polymers 0.000 description 4
- 229920002521 macromolecule Polymers 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 239000002023 wood Substances 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000000446 fuel Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 108091005804 Peptidases Proteins 0.000 description 1
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- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 229920001436 collagen Polymers 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
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- 238000000354 decomposition reaction Methods 0.000 description 1
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- 229910001873 dinitrogen Inorganic materials 0.000 description 1
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- 210000001723 extracellular space Anatomy 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2307/00—Characterised by the use of natural rubber
Abstract
The invention belongs to the technical field of rubber production, and particularly relates to an industrial production process of eucommia ulmoides rubber. The industrial production process of the eucommia ulmoides rubber provided by the invention comprises the following steps: (1) peeling eucommia seed; (2) performing enzymolysis on eucommia seed peels; (3) solvent extraction; (4) separating glue solution; (5) settling the glue solution; (6) coagulating the glue solution; (7) separating the glue solution from the solvent; (8) drying the eucommia ulmoides gum. The invention adopts a specific process and combines specific equipment, so that the whole process of extracting the gutta-percha is green and environment-friendly, the production efficiency is high, the product purity is high, the production cost is low, the arrangement among the working procedures is reasonable, the connection is compact, and the industrialization of the gutta-percha production is realized.
Description
Technical Field
The invention belongs to the technical field of rubber production, and particularly relates to an industrial production process of eucommia ulmoides rubber.
Background
Eucommia bark is an important collagen plant, and leaves, barks and seed barks are all rich in a white filamentous substance, namely eucommia bark gum. The following patent documents disclose methods for extracting gutta percha:
CN104356398A discloses a method for extracting gutta-percha by a whole biological enzyme method, which comprises the steps of firstly blasting and cracking eucommia bark which is taken as a raw material, then sequentially using protease to decompose protein components in the eucommia bark, using pectinase to decompose intercellular walls and intercellular spaces in the eucommia bark, using cellulase to improve the decomposition of cellulose and hemicellulose, thereby decomposing non-glue substances in the eucommia bark into components which can be completely separated from the gutta-percha, and using a method of rotating a separation cylinder in an extraction kettle in a water tank to separate a target object from waste components, wherein the inner wall of the separation cylinder is provided with a bent plate stirring blade with an angular cross section, the included angle of the bent plate is not less than 120 degrees, the stirring blade and a support shaft form an inclined angle of 10-15 degrees, and the bent plate is provided with an elongated hole in a staggered manner, so that the thoroughness of separation of the target object and the waste components is ensured, low cost and high efficiency, and the purity of the extracted gutta-percha is high and can reach more than 92 percent, thus being suitable for industrialized production.
The above process has the disadvantages of long enzymolysis time, each time of enzyme action time is 28-32 h, and the enzymolysis time is shortened to 6-8h by adopting vertical enzymolysis.
Therefore, it is necessary to improve the above process, and design a set of equipment for the new and improved process to meet the requirements of the new process.
Disclosure of Invention
In order to solve the technical problems, the invention provides an industrial production process of the eucommia ulmoides rubber, which has high production efficiency, high product purity and low production cost;
meanwhile, the invention also provides equipment matched with the process.
The invention mainly takes the husked eucommia seed peels as main raw materials, firstly carries out enzymolysis to obtain eucommia crude gum, then adopts the scheme of solvent extraction to obtain eucommia gum liquid, and then carries out the processes of separation, sedimentation, agglomeration, drying and the like to obtain the high-purity bio-based eucommia polymer material, and the husked seed kang can be used as bio-based fuel for further recycling.
The industrial production process of the eucommia ulmoides rubber comprises the following steps:
(1) husking eucommia seeds: husking eucommia seeds, and separating seed husks and seed kernels, wherein the seed husks are used as raw materials for extracting eucommia rubber for later use;
(2) enzymolysis of eucommia seed peels: taking the seed peels in the step (1), and respectively carrying out enzymolysis on the seed peels in an extraction kettle by adopting cellulase, pectinase and acid protease;
(3) extraction: adding an organic solvent into the enzymatic hydrolysate obtained in the step (2) for extraction;
(4) glue solution separation: separating glue solution and glue residue by adopting glue residue filtering equipment;
(5) and (3) glue solution sedimentation: settling the separated glue solution, and purifying the glue solution;
(6) and (3) coagulating glue liquid: freezing the glue solution at ultralow temperature to condense the eucommia ulmoides gum from the glue solution;
(7) separating glue solution from solvent: centrifugally separating the glue solution from the rubber particles;
(8) drying the eucommia ulmoides gum: drying gutta-percha at low temperature by using nitrogen as a protective agent.
Preferably, in the step (2), the addition amount of the cellulase, the pectinase and the acid protease is 1.2-1.5% of the addition amount of the seed husk respectively; the enzymolysis temperature is 45-70 ℃, and the total enzymolysis time is 12-24 h; and (3) inactivating enzyme for 5-15 min at 95-100 ℃ after enzymolysis.
Preferably, the organic solvent in the step (3) is petroleum ether, and the adding amount of the petroleum ether is 15-20 times of the mass of the raw material seed husk.
(3) The temperature of the medium solvent is controlled to be 50-80 ℃ during extraction, and the extraction time is 30-60 min.
(4) Drying the separated rubber slag and recovering the rubber solution.
Preferably, in (4), the separated skim latex is dried, the latex is recovered, and the recovered latex is combined with the latex obtained by separation.
(6) And in the middle and ultra-low temperature freezing, the temperature is controlled to be-20 to-10 ℃.
(8) In the method, low-temperature drying is carried out at the temperature of-10 to 5 ℃; drying at low temperature until the moisture content is reduced to 0.2-0.8%.
The industrial production process of the eucommia ulmoides rubber comprises the following steps:
(1) husking eucommia seeds: husking eucommia seeds, and separating seed husks and seed kernels, wherein the seed husks are used as raw materials for extracting eucommia rubber for later use;
(2) enzymolysis of eucommia seed peels: taking the seed peels in the step (1), and respectively carrying out enzymolysis on the seed peels in an extraction kettle by adopting cellulase, pectinase and acid protease; the enzymolysis temperature is 45-70 ℃, and the total enzymolysis time is 12-24 h; inactivating enzyme at 95-100 ℃ for 5-15 min after enzymolysis;
(3) extraction: adding an organic solvent petroleum ether into the enzymolysis liquid in the step (1) for extraction; the dosage of the petroleum ether is 15-20 times of the mass of the raw material seed husk; the temperature is controlled to be 50-80 ℃ during extraction, and the extraction time is 30-60 min;
(4) glue solution separation: separating glue solution and glue residue by adopting glue residue filtering equipment;
(5) and (3) glue solution sedimentation: settling the separated glue solution, and purifying the glue solution; adding a flocculating agent during purification, and combining wood residues in the glue solution with macromolecules of the flocculating agent by adopting a flocculation method so as to settle to the bottom of the tank body and separate from the glue solution, so that the glue solution is purified;
(6) and (3) coagulating glue liquid: freezing the glue solution obtained in the step (5) at an ultralow temperature of between 20 ℃ below zero and 10 ℃ below zero to condense the eucommia ulmoides gum from the glue solution;
(7) separating glue solution from solvent: centrifugally separating the glue solution from the rubber particles;
(8) drying the eucommia ulmoides gum: and drying the eucommia ulmoides gum at a low temperature of-10-5 ℃ by taking nitrogen as a protective agent until the moisture content is reduced to 0.2-0.8%.
The device comprises a solvent tank, wherein the solvent tank is connected with an extraction kettle through a pipeline, and the extraction kettle is sequentially connected with a separator, a glue solution tank, a settling tank, a condensation kettle, a centrifuge and a solvent cache tank;
the settling tank comprises a first settling tank and a second settling tank which are connected in parallel; the pipeline connected with the outlet of the glue solution tank is divided into two branches, one branch is communicated with the first settling tank, the other branch is communicated with the second settling tank, and the first settling tank and the pipeline at the bottom of the second settling tank are converged and then are led to the condensation kettle;
the condensation kettle comprises a first condensation kettle and a second condensation kettle which are connected in parallel; the pipeline connected with the outlet of the settling tank is divided into two branches, one branch is communicated with the first coagulation kettle, the other branch is communicated with the second coagulation kettle, and the pipelines at the bottoms of the first coagulation kettle and the second coagulation kettle are converged and then lead to the centrifugal machine; the centrifuge is also connected with a dry material pipeline, and materials in the dry material pipeline are led to the drying device.
The pipeline that is connected with the export of solvent buffer tank carries the material to the solvent jar to realize the recovery and the reuse of solvent.
The solvent tank and the extraction kettle are provided with a first delivery pump, a second delivery pump is arranged between the glue solution tank and the settling tank, a third delivery pump is arranged between the settling tank and the condensation kettle, and a fourth delivery pump is arranged on a pipeline connected with an outlet of the solvent cache tank.
The invention adopts unique production process and equipment, the whole process is environment-friendly, the production efficiency is high, the product purity is high, the production cost is low, the arrangement among the working procedures is reasonable, the connection is compact, the invention is the most advanced technology for extracting the gutta-percha at present, and the industrialization of the gutta-percha production is realized.
The invention has the beneficial effects that:
(1) when the eucommia seeds are peeled, the invention adopts specific equipment, can efficiently separate the eucommia seed kernels from the hard seed shells, and can continuously operate for 24 hours. The kernel yield and the seed peel yield respectively reach 27 percent and 26 percent, and a foundation is laid for the subsequent extraction work;
(2) specific enzyme is adopted to carry out enzymolysis on the eucommia seed skin, the enzymolysis efficiency is greatly improved, and the enzymolysis cost is reduced by more than 80%;
(3) in the step of separating the glue solution from the glue residues, the glue solution in the glue residues is recycled, so that the obtaining amount of the glue solution is greatly increased, and the subsequent extraction amount of the eucommia ulmoides rubber is increased;
(4) when the eucommia ulmoides rubber is dried, nitrogen is used as a protective agent, rubber is prevented from being oxidized, the drying temperature is controlled within a reasonable range, low-temperature rapid drying is realized, and the quality of the eucommia ulmoides rubber is ensured.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a view showing the construction of an extracting apparatus of the present invention;
in the figure, 1-solvent tank, 2-delivery pump, 3-extraction kettle, 4-separator, 5-glue solution tank, 6-first settling tank, 61-second settling tank, 7-first coagulation kettle, 71-second coagulation kettle, 8-centrifuge, 9-solvent buffer tank.
Detailed Description
The present invention will be further described with reference to specific examples so that those skilled in the art may better understand the present invention, but the present invention is not limited thereto.
Example 1
The extraction equipment used in the industrial production process of the eucommia ulmoides rubber comprises the following structures: the extraction equipment comprises a solvent tank 1, the solvent tank 1 is connected with an extraction kettle 3 through a pipeline, and the extraction kettle 3 is sequentially connected with a separator 4, a glue solution tank 5, a settling tank, a coagulation kettle, a centrifuge 8 and a solvent buffer tank 9;
the settling tank comprises a first settling tank 6 and a second settling tank 61, and the first settling tank 6 and the second settling tank 61 are connected in parallel; the pipeline connected with the outlet of the glue solution tank 5 is divided into two branches, one branch is communicated with the first settling tank 6, the other branch is communicated with the second settling tank 61, and the pipelines at the bottoms of the first settling tank 6 and the second settling tank 61 are converged and then led to the condensation kettle;
the condensation kettle comprises a first condensation kettle 7 and a second condensation kettle 71, and the first condensation kettle 7 and the second condensation kettle 71 are connected in parallel; the pipeline connected with the outlet of the settling tank is divided into two branches, one branch is communicated with the first coagulation kettle 7, the other branch is communicated with the second coagulation kettle 71, and the pipelines at the bottoms of the first coagulation kettle 7 and the second coagulation kettle 71 are converged and then led to the centrifuge 8; the centrifuge 8 is also connected with a dry material pipeline, and the material in the dry material pipeline is led to a drying device.
The outlet of the centrifuge 8 is connected with the inlet of the solvent buffer tank 9; a pipe connected to the outlet of the solvent buffer tank 9 transports the material to the solvent tank.
The solvent tank 1 and the extraction kettle 3 are provided with a first delivery pump 201, a second delivery pump 202 is arranged between the glue solution tank 5 and the settling tank, a third delivery pump 203 is arranged between the settling tank and the condensation kettle, and a fourth delivery pump 204 is arranged on a pipeline connected with the outlet of the solvent buffer tank 9.
The structure of the extraction kettle is as follows: a feed inlet 301 is arranged on one side of the upper part of the extraction kettle 3 main body, and a discharge outlet 302 is arranged at the bottom; the upper part of the main body of the extraction kettle 3 is provided with a stirring motor 303, the stirring motor 303 is connected with a rotating shaft 305 of a stirring paddle 304, and after the power is on, the motor 303 drives the rotating shaft 305 of the stirring paddle 304 to rotate so as to rotate the stirring paddle 304; the bottom of the extraction kettle 3 is provided with a shutter 306, and the upper part of the shutter 306 is provided with a filter screen 308. A manhole 308 is arranged on the other side of the upper part of the extraction kettle 3 main body; of course, the main body of the extraction kettle 3 is also provided with an air release port and an air release valve, and similar conventional designs can be set according to specific conditions.
The filter screen 308 is a 200-mesh filter screen; the paddle 304 is an anchor paddle.
The industrial production of the eucommia rubber is realized by utilizing the equipment, and the specific process is as follows:
peeling eucommia seeds, separating seed husks and seed kernels, taking the seed husks as a raw material for extracting eucommia rubber, putting the seed husks into an extraction kettle 3, adding compound enzymes, performing enzymolysis extraction for a certain time, pumping a solvent in a solvent tank 1 into the extraction kettle 3 after the enzymolysis extraction is finished, and performing action on enzymolysis liquid through the solvent for further extraction; then, conveying the extracted materials into a separator 4, separating glue solution from glue residues, and settling the glue solution by using a first settling tank 6 and a second settling tank 61 after separation; then the settled gum solution is frozen at ultra-low temperature by a first condensation kettle 7 and a second condensation kettle 71 to condense the gutta-percha from the gum solution; the gum solution and rubber particles are centrifugally separated by a centrifuge 8, and then the gutta percha is dried at low temperature under the condition that nitrogen is used as a protective agent.
Meanwhile, the solvent in the centrifuge 8 enters a solvent buffer tank 9, and is recycled and then enters the tank 1 for continuous recycling.
Example 2
The industrial production process of the eucommia ulmoides rubber comprises the following steps:
(1) husking eucommia seeds: husking eucommia seeds, and separating seed husks and seed kernels, wherein the seed husks are used as raw materials for extracting eucommia rubber for later use; wherein, the seed kernels are extruded and granulated to be used as bio-based fuel;
(2) enzymolysis of eucommia seed peels: taking the seed peels in the step (1), and respectively carrying out enzymolysis on the seed peels in an extraction kettle by adopting cellulase, pectinase and acid protease; the enzymolysis temperature is about 55 ℃, and the total enzymolysis time is 16 h; inactivating enzyme at 95 deg.C for 5min after enzymolysis;
(3) extraction: adding an organic solvent petroleum ether into the enzymolysis liquid in the step (1) for extraction; the dosage of the petroleum ether is 18 times of the mass of the raw material seed coat; the extraction temperature is controlled at 70 deg.C, and the extraction time is 40 min;
(4) glue solution separation: separating glue solution and glue residue by adopting glue residue filtering equipment;
(5) and (3) glue solution sedimentation: settling the separated glue solution, and purifying the glue solution; adding a flocculating agent during purification, and combining wood residues in the glue solution with macromolecules of the flocculating agent by adopting a flocculation method so as to settle to the bottom of the tank body and separate from the glue solution, so that the glue solution is purified;
(6) and (3) coagulating glue liquid: freezing the glue solution obtained in the step (5) at an ultralow temperature of-15 ℃ to enable the eucommia ulmoides gum to be condensed from the glue solution;
(7) separating glue solution from solvent: centrifugally separating the glue solution from the rubber particles;
(8) drying the eucommia ulmoides gum: and drying the eucommia ulmoides gum particles at a low temperature of-8 ℃ by taking nitrogen as a protective agent until the moisture content is reduced to 0.5 percent to obtain the finished product eucommia ulmoides rubber.
In the process, the organic solvent in the centrifugal supernatant is recovered and recycled.
Example 3
The industrial production process of the eucommia ulmoides rubber comprises the following steps:
(1) husking eucommia seeds: husking eucommia seeds, and separating seed husks and seed kernels, wherein the seed husks are used as raw materials for extracting eucommia rubber for later use;
(2) enzymolysis of eucommia seed peels: taking the seed peels in the step (1), and respectively carrying out enzymolysis on the seed peels in an extraction kettle by adopting cellulase, pectinase and acid protease; the enzymolysis temperature is 50 ℃, and the total enzymolysis time is 18 h; inactivating enzyme at 95 deg.C for 10min after enzymolysis;
(3) extraction: adding an organic solvent petroleum ether into the enzymolysis liquid in the step (1) for extraction; the dosage of the petroleum ether is 16 times of the mass of the raw material seed husk; the extraction temperature is controlled at 60 deg.C, and the extraction time is 45 min;
(4) glue solution separation: separating glue solution and glue residue by adopting glue residue filtering equipment;
(5) and (3) glue solution sedimentation: settling the separated glue solution, and purifying the glue solution; adding a flocculating agent during purification, and combining wood residues in the glue solution with macromolecules of the flocculating agent by adopting a flocculation method so as to settle to the bottom of the tank body and separate from the glue solution, so that the glue solution is purified;
(6) and (3) coagulating glue liquid: freezing the glue solution obtained in the step (5) at an ultralow temperature of-10 ℃ to enable the eucommia ulmoides gum to be condensed out from the glue solution;
(7) separating glue solution from solvent: centrifugally separating the glue solution from the rubber particles;
(8) drying the eucommia ulmoides gum: nitrogen gas is used as a protective agent, and the eucommia ulmoides gum is dried at low temperature of-2 ℃ until the moisture content is reduced to 0.6 percent.
Example 4
The industrial production process of the eucommia ulmoides rubber comprises the following steps:
(1) husking eucommia seeds: husking eucommia seeds, and separating seed husks and seed kernels, wherein the seed husks are used as raw materials for extracting eucommia rubber for later use;
(2) enzymolysis of eucommia seed peels: taking the seed peels in the step (1), and respectively carrying out enzymolysis on the seed peels in an extraction kettle by adopting cellulase, pectinase and acid protease; the enzymolysis temperature is 45 ℃, and the total enzymolysis time is 12 h; inactivating enzyme at 100 deg.C for 5min after enzymolysis;
(3) extraction: adding an organic solvent petroleum ether into the enzymolysis liquid in the step (1) for extraction; the dosage of the petroleum ether is 15 times of the mass of the raw material seed coat; the extraction temperature is controlled at 60 deg.C, and the extraction time is 50 min;
(4) glue solution separation: separating glue solution and glue residue by adopting glue residue filtering equipment;
(5) and (3) glue solution sedimentation: settling the separated glue solution, and purifying the glue solution; adding a flocculating agent during purification, and combining wood residues in the glue solution with macromolecules of the flocculating agent by adopting a flocculation method so as to settle to the bottom of the tank body and separate from the glue solution, so that the glue solution is purified;
(6) and (3) coagulating glue liquid: freezing the glue solution obtained in the step (5) at an ultralow temperature of-15 ℃ to enable the eucommia ulmoides gum to be condensed from the glue solution;
(7) separating glue solution from solvent: centrifugally separating the glue solution from the rubber particles;
(8) drying the eucommia ulmoides gum: and drying the eucommia ulmoides gum at a low temperature of-5 ℃ by taking nitrogen as a protective agent until the moisture content is reduced to 0.2-0.8%.
Example 5
The detection results of the eucommia ulmoides rubber obtained in the embodiments 2-4 show that the extraction rate of the eucommia ulmoides rubber is more than 95%, and the purity of the eucommia ulmoides rubber is more than or equal to 99%. The finished rubber product is inspected, and the Mooney viscosity of the rubber product is 90 +/-15, the 300% stress at definite elongation is 20.1 +/-2.0 MPa, the tensile strength is more than or equal to 25.0MPa, and the elongation at break is more than or equal to 35 percent. The application standard of the rubber is reached.
The detection method of the extraction rate comprises the following steps: extraction rate = gutta percha dry weight/gutta percha weight actually contained in the sample × 100%;
the purity detection method comprises the following steps: chromic acid oxidation method (rubber industry handbook, edition group, sixth booklet, Up book; Beijing: chemical industry Press)
The different batches of samples produced at different times chosen by the inventors are as follows:
note: in the above tables, the extraction rates in numbers 1-3 are the same, i.e., they are different samples of the same batch; the extraction rates of numbers 1 and 4 were different, i.e. they were different samples of different batches.
From the above tables, it can be seen that the extraction rate of the eucommia ulmoides rubber is high, which reaches about 96.4% at most, and the 300% stress at definite elongation, tensile strength and elongation are all ideal, and reach the application standard of rubber.
Besides obtaining high-quality eucommia ulmoides rubber, the process realizes large-scale continuous production, shortens the time and improves the production efficiency.
Claims (10)
1. The industrial production process of the eucommia ulmoides rubber comprises the following steps:
(1) husking eucommia seeds: husking eucommia seeds, and separating seed husks and seed kernels, wherein the seed husks are used as raw materials for extracting eucommia rubber for later use;
(2) enzymolysis of eucommia seed peels: taking the seed peels in the step (1), and respectively carrying out enzymolysis on the seed peels in an extraction kettle by adopting cellulase, pectinase and acid protease;
(3) extraction: adding an organic solvent into the enzymolysis liquid obtained in the step (2) for extraction;
(4) glue solution separation: separating glue solution and glue residue by adopting glue residue filtering equipment;
(5) and (3) glue solution sedimentation: settling the separated glue solution, and purifying the glue solution;
(6) and (3) coagulating glue liquid: freezing the glue solution at ultralow temperature to condense the eucommia ulmoides gum from the glue solution;
(7) separating glue solution from solvent: centrifugally separating the glue solution from the rubber particles;
(8) drying the eucommia ulmoides gum: drying gutta-percha at low temperature by using nitrogen as a protective agent.
2. The industrial production process of eucommia ulmoides rubber as claimed in claim 1, wherein in the step (2), the addition amounts of the cellulase, the pectinase and the acid protease are 1.2-1.5% of the addition amount of the seed husk respectively; the enzymolysis temperature is 45-70 ℃, and the total enzymolysis time is 12-24 h; and (3) inactivating enzyme for 5-15 min at 95-100 ℃ after enzymolysis.
3. The industrial production process of eucommia ulmoides rubber as claimed in claim 1, wherein in the step (3), the organic solvent is petroleum ether, and the addition amount of the petroleum ether is 15-20 times of the mass of the raw material seed skin.
4. The industrial production process of eucommia ulmoides rubber as claimed in claim 1, wherein the temperature of the solvent extraction in the step (3) is controlled to be 50-80 ℃ and the extraction time is 30-60 min.
5. The process for industrially producing eucommia ulmoides rubber according to claim 1, wherein in (4), the separated pomace is dried and the cement is recovered.
6. The process for industrially producing eucommia ulmoides rubber according to claim 1, wherein in (4), the separated pomace is dried, the gum solution is recovered, and the recovered gum solution is combined with the gum solution obtained by separation.
7. The industrial production process of eucommia ulmoides rubber as claimed in claim 1, wherein in (6), the temperature is controlled at-20 to-10 ℃ during ultra-low temperature freezing.
8. The industrial production process of eucommia ulmoides rubber as claimed in claim 1, wherein in (8), the low temperature drying is performed at-10 to 5 ℃; drying at low temperature until the moisture content is reduced to 0.2-0.8%.
9. The industrial production process of eucommia ulmoides rubber as claimed in claim 1, comprising the steps of:
(1) husking eucommia seeds: husking eucommia seeds, and separating seed husks and seed kernels, wherein the seed husks are used as raw materials for extracting eucommia rubber for later use;
(2) enzymolysis of eucommia seed peels: taking the seed peels in the step (1), and respectively carrying out enzymolysis on the seed peels in an extraction kettle by adopting cellulase, pectinase and acid protease; the enzymolysis temperature is 45-70 ℃, and the total enzymolysis time is 12-24 h; inactivating enzyme at 95-100 ℃ for 5-15 min after enzymolysis;
(3) extraction: adding an organic solvent petroleum ether into the enzymolysis liquid obtained in the step (2) for extraction; the dosage of the petroleum ether is 15-20 times of the mass of the raw material seed husk; the temperature is controlled to be 50-80 ℃ during extraction, and the extraction time is 30-60 min;
(4) glue solution separation: separating glue solution and glue residue by adopting glue residue filtering equipment;
(5) and (3) glue solution sedimentation: settling the separated glue solution, and purifying the glue solution;
(6) and (3) coagulating glue liquid: freezing the glue solution obtained in the step (5) at an ultralow temperature of between 20 ℃ below zero and 10 ℃ below zero to condense the eucommia ulmoides gum from the glue solution;
(7) separating glue solution from solvent: centrifugally separating the glue solution from the rubber particles;
(8) drying the eucommia ulmoides gum: and drying the eucommia ulmoides gum at a low temperature of-10-5 ℃ by taking nitrogen as a protective agent until the moisture content is reduced to 0.2-0.8%.
10. The apparatus for the industrial production process of gutta percha as the claim 1, wherein said apparatus comprises a solvent tank (1), said solvent tank (1) is connected with an extraction pot (3) through a pipe, said extraction pot (3) is connected with a separator (4), a glue solution tank (5), a settling tank, a coagulation pot, a centrifuge (8), a solvent buffer tank (9) in turn;
the settling tank comprises a first settling tank (6) and a second settling tank (61), and the first settling tank (6) and the second settling tank (61) are connected in parallel; the pipeline connected with the outlet of the glue solution tank (5) is divided into two branches, one branch is communicated with the first settling tank (6), the other branch is communicated with the second settling tank (61), and the first settling tank (6) and the pipeline at the bottom of the second settling tank (61) are converged and then led to the condensation kettle;
the condensation kettle comprises a first condensation kettle (7) and a second condensation kettle (71), and the first condensation kettle (7) and the second condensation kettle (71) are connected in parallel; the pipeline connected with the outlet of the settling tank is divided into two branches, one branch is communicated with the first condensation kettle (7), the other branch is communicated with the second condensation kettle (71), and the pipelines at the bottoms of the first condensation kettle (7) and the second condensation kettle (71) are converged and then led to the centrifuge (8); the centrifugal machine (8) is also connected with a drying material pipeline, and materials in the drying material pipeline are led to the drying device.
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