CN112812888A - Lacquer seed oil dewaxing and production process - Google Patents
Lacquer seed oil dewaxing and production process Download PDFInfo
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- CN112812888A CN112812888A CN202011613335.2A CN202011613335A CN112812888A CN 112812888 A CN112812888 A CN 112812888A CN 202011613335 A CN202011613335 A CN 202011613335A CN 112812888 A CN112812888 A CN 112812888A
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- 239000004922 lacquer Substances 0.000 title claims abstract description 279
- 235000015112 vegetable and seed oil Nutrition 0.000 title claims abstract description 158
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 239000013078 crystal Substances 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 38
- 238000000926 separation method Methods 0.000 claims abstract description 18
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 238000010583 slow cooling Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 48
- 238000007670 refining Methods 0.000 claims description 45
- 238000003756 stirring Methods 0.000 claims description 40
- 238000010438 heat treatment Methods 0.000 claims description 34
- 238000003825 pressing Methods 0.000 claims description 24
- 230000018044 dehydration Effects 0.000 claims description 17
- 238000006297 dehydration reaction Methods 0.000 claims description 17
- 238000004042 decolorization Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 238000004332 deodorization Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- 230000001877 deodorizing effect Effects 0.000 claims description 9
- 238000007599 discharging Methods 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 8
- 239000003153 chemical reaction reagent Substances 0.000 claims description 6
- 235000019362 perlite Nutrition 0.000 claims description 6
- 239000010451 perlite Substances 0.000 claims description 6
- 230000001376 precipitating effect Effects 0.000 claims description 6
- 235000012771 pancakes Nutrition 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 3
- 238000011946 reduction process Methods 0.000 claims description 3
- 235000019198 oils Nutrition 0.000 abstract description 10
- 230000003450 growing effect Effects 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 description 12
- 239000000463 material Substances 0.000 description 10
- 239000000047 product Substances 0.000 description 8
- 239000007921 spray Substances 0.000 description 6
- 238000001914 filtration Methods 0.000 description 4
- 238000007710 freezing Methods 0.000 description 4
- 230000008014 freezing Effects 0.000 description 4
- 238000002791 soaking Methods 0.000 description 3
- 244000044283 Toxicodendron succedaneum Species 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000003910 Baronia <angiosperm> Species 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B7/00—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils
- C11B7/0075—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils by differences of melting or solidifying points
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Microbiology (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention provides a lacquer seed oil dewaxing and production process, which mainly solves the problems of incomplete oil-wax separation and high production cost in lacquer seed oil production in the prior art. When the technical scheme provided by the invention is used for preparing the lacquer seed oil or dewaxing the lacquer seed oil, the efficiency is high, the cost is low, the oil and wax separation is very thorough, and the wax content is lower than 2%. The lacquer seed oil dewaxing and production process provided by the invention can be directly applied to industrial streamlined production, so that the yield of high-quality lacquer seed oil is greatly improved, and the lacquer seed oil produced by the method has longer storage time. According to the invention, by controlling the multi-gradient and long-time slow cooling process, the more uniform the cooling process is, the better the crystal growing effect is, the temperature can be reduced by about 0.1 ℃ per ten minutes averagely in the cooling link, and the lacquer wax in the lacquer seed oil can be separated out as much as possible by the high-precision control, so that the yield of the lacquer wax is improved, the purity of the lacquer seed oil is improved, and the industrial production is facilitated.
Description
Technical Field
The invention relates to a dewaxing and production process, in particular to a lacquer seed oil dewaxing and production process.
Background
The fruit of lacquer tree is also called lacquer seed, is in flat oblique spherical shape, is similar to soybean in size, and is collected in 9-10 months in autumn every year. The pericarp is divided into 3 layers, the epicarp is gray yellow or yellow green, the middle pulp is wax layer, and is light yellow or gray green to extract lacquer wax. The kernel is seed and can be used for squeezing lacquer oil. The oil content, chemical composition and physical characteristics of the lacquer seeds are different due to different tree varieties, and the oil content of the lacquer seeds of Rhus Succedanea (Rhus sucedenanea L) is about 2-8%.
CN201210201032.9 discloses a method for extracting lacquer seed oil, which mainly comprises the following steps: 1) screening fresh lacquer seeds, removing impurities, and drying at a temperature not higher than 60 ℃; 2) pulverizing dried lacquer seed at a temperature of not higher than 20 deg.C; 3) soaking the crushed lacquer seed powder in water, stirring and separating into a lacquer seed kernel sinking to the water bottom layer, and lacquer seed skin and fruit pulp floating on the upper part of the water; 4) collecting the separated lacquer seed kernel, freezing and crushing to obtain a lacquer seed kernel crushed object, wherein the temperature is controlled to be not higher than 10 ℃ in the crushing process after the lacquer seed kernel is frozen; before freezing, centrifugal separation is carried out to remove water; the freezing temperature is-10 to-20 ℃; 5) steaming the crushed lacquer seed inner core for 15-45 min at 100-102 ℃; 6) squeezing the crushed material of the inner core of the cooked lacquer seed; carrying out ultrasonic stirring and decoloring treatment on the squeezed lacquer seed oil solution to obtain a finished product; 6) the squeezing pressure in the step is 5-6 Mpa; 6) the decolorization in the step is that the squeezed lacquer seed oil solution is pumped into a decolorization tank for decolorization; controlling the temperature to be 70-80 ℃, stirring by using a stirrer, and beating by using ultrasonic waves; 6) the stirring speed in the step is 50-60rpm, the ultrasonic power and the frequency are respectively 400W and 47.6kHz, the treatment is carried out for 60-70min, and the separation is carried out.
The method for preparing the lacquer seed oil has the following problems:
1. the oil-wax separation is not thorough, so that the wax content in the lacquer seed oil is high, and the use of the lacquer seed oil is influenced;
2. the cost is higher by adopting a freezing mode;
therefore, it is highly desirable to provide a dewaxing and production process for lacquer seed oil, which can completely complete the oil-wax separation and reduce the cost.
Disclosure of Invention
The invention provides a lacquer seed oil dewaxing and production process, which mainly solves the problems of incomplete oil-wax separation and high production cost in lacquer seed oil production in the prior art.
The specific technical solution of the invention is as follows:
the invention can perform finish dewaxing on semi-finished product lacquer seed oil (crude lacquer seed oil) with high wax content, and can also directly prepare high-quality lacquer seed oil from lacquer seed kernels.
If the lacquer seed kernel is directly processed into high-quality lacquer seed oil, the method comprises the following steps:
1 ] preparation of crude Lacquer seed oil
1.1, putting the lacquer seed nucleolus in alkaline water with the temperature of 80-90 ℃ and the pH value of 10-12, stirring for 20-40 min, removing a wax layer on the surface of the lacquer seed nucleolus, and taking out the lacquer seed nucleolus after stirring;
1.2, placing the lacquer seed nucleolus processed in the step 1.1 in hot water at the temperature of 80-90 ℃ to be stirred for 20-40 min again, removing the residual wax coat on the surface of the lacquer seed nucleolus, and taking out the lacquer seed nucleolus after stirring;
1.3, drying the lacquer seed kernels treated in the step 1.2 at the temperature of 70-80 ℃ for 50-70 min, removing water on the surfaces of the lacquer seed kernels, crushing the lacquer seed kernels to 20-40 meshes after the water is removed, and pressing the milled lacquer seed kernels into a pancake shape of 1-3 mm;
1.4, drying the thin-cake-shaped lacquer seed kernels processed in the step 1.3 again for 50-70 min at the temperature of 90-100 ℃ to reduce the water content of the lacquer seed kernels to below 2%;
1.5, squeezing the pancake-shaped lacquer seed kernels processed in the step 1.4 to obtain crude lacquer seed oil;
degumming, deacidification and decolorization
Degumming, deacidifying and decolorizing the crude lacquer seed oil at 70-90 ℃;
3 dewaxing by growing crystals
Carrying out dewaxing treatment on the lacquer seed oil treated in the step 1:
3.1, slowly reducing the temperature of the lacquer seed oil from 55 +/-3 ℃ to 35 +/-3 ℃ within 20-30 hours, and separating out lacquer wax crystals growing to 0.3-0.7 mm in the temperature reduction process;
3.2, slowly reducing the temperature of the lacquer seed oil from the temperature at the end of the step 3.1 to 8 +/-3 ℃ within 6-15 hours, and continuously precipitating lacquer wax crystals to grow to 1.2-2.2 mm;
3.3, preserving the heat for 3-6 hours in the temperature environment at the end of the step 3.2, and further precipitating lacquer wax crystals to grow to 2.8-3.6 mm; (ii) a
3.4, adding a filter aid accounting for 1.5 to 2.5 percent of the weight of the lacquer seed oil into the lacquer seed oil in the temperature environment at the end of the step 3.3, and stirring for 50 to 80min under heat preservation;
3.5, performing oil-wax separation on the lacquer seed oil treated in the step 3.4, and separating lacquer wax crystals;
4 ] deodorization and dehydration
And (3) deodorizing and dehydrating the lacquer seed oil obtained by the treatment in the step (2) to obtain the finished product lacquer seed oil.
If finishing is performed on the semi-finished lacquer seed oil (crude lacquer seed oil), it is possible to start directly from step 2.
Further, in step 2, the crude lacquer seed oil is degummed, deacidified and decolored at 80 ℃.
Further, in step 3.1 ], the temperature of the lacquer seed oil is reduced from 50 ℃ to 35 ℃.
Further, in step 3.2 ], the temperature is lowered to 10 ℃.
Further, in step 3.3 ], the filter aid is perlite.
The core of the invention lies in the slow cooling described in the steps 3.1 and 3.2, the control process of the slow cooling is relatively complex, and the control process is specifically realized by adopting a refining tank, wherein the refining tank 3 comprises a refining tank body 32 on a refining tank support frame 31, a first stirrer 39 is arranged in the refining tank body 32, the top of the refining tank body 32 is connected with a water inlet pipe 33 and a reagent unit 34, the side wall of the refining tank body 32 is provided with a feeding pipe 35, and the bottom of the refining tank body 32 is connected with one end of a discharging pipe 36 and an impurity discharging pipe 37; the refining tank body 32 is also provided with a third heating unit 38; the third heating unit 38 is a heating coil wound around the tank, and liquid is introduced into the heating coil to control the cooling process.
The invention has the advantages that:
1. when the technical scheme provided by the invention is used for preparing the lacquer seed oil or dewaxing the lacquer seed oil, the efficiency is high, the cost is low, the oil and wax separation is very thorough, and the wax content is lower than 2%.
2. The lacquer seed oil dewaxing and production process provided by the invention can be directly applied to industrial streamlined production, so that the yield of high-quality lacquer seed oil is greatly improved, and the lacquer seed oil produced by the method has longer storage time.
3. According to the invention, by controlling the multi-gradient and long-time slow cooling process, the more uniform the cooling process is, the better the crystal growing effect is, the temperature can be reduced by about 0.1 ℃ per ten minutes averagely in the cooling link, and the lacquer wax in the lacquer seed oil can be separated out as much as possible by the high-precision control, so that the yield of the lacquer wax is improved, the purity of the lacquer seed oil is improved, and the industrial production is facilitated.
Drawings
FIG. 1 is a schematic structural view of the present invention;
the drawings are as follows:
the device comprises a rough-making tank 1, a pressing tank 2, a refining tank 3, a dewatering tank 4, a vacuumizing unit 5, a temperature detection unit 6, a pressure detection unit 7, a material receiving unit 8, a rough-making tank support frame 11, a rough-making tank body 12, a spiral stirrer 13, a filter screen 14, an alkali water spray pipe 15, a clear water spray pipe 16, a liquid discharge port 17, a first heating unit 18, a rough material outlet 19, a pressing tank body 21, a T-shaped extrusion plate 22, a filter plate 23, a second heating unit 24, a pressed oil outlet 25, a guide plate 26, a refining tank support frame 31, a refining tank body 32, a water inlet pipe 33, a reagent unit 34, a material inlet pipe 35, a material outlet pipe 36, a impurity discharge pipe 37, a third heating unit 38, a first stirrer 39, a dewatering tank support frame 41, a dewatering tank body 42, a second stirrer 43, a material discharge pipe 44 and a fourth heating unit 45.
Detailed Description
The core of the invention lies in the selection of dewaxing time point, the fine control of temperature in the processes of alkaline water leaching and crystal growing dewaxing, in the existing production process, the production of lacquer seed oil is mostly that the lacquer seed kernel is heated and crushed firstly, skin and meat are separated after the heating and crushing are finished, and then the lacquer seed kernel is cooked and squeezed after being frozen and crushed for the second time; the invention is cooked and then squeezed, and then the lacquer wax crystal is fully separated out through temperature control, so the process design is more reasonable, and the cost is lower.
The invention is described in detail below with reference to specific examples:
example one
Degumming, deacidification and decolorization
Degumming, deacidifying and decolorizing the crude lacquer seed oil at 70 ℃;
crystal growth dewaxing
Carrying out dewaxing treatment on the lacquer seed oil treated in the step 1:
2.1, reducing the temperature of the lacquer seed oil from 55 ℃ to 35 ℃ within 30 hours, and enabling lacquer wax crystals to grow to 0.7 mm;
2.2 reducing the temperature of the lacquer seed oil to 10 ℃ within 10 hours, and enabling lacquer wax crystals to grow to 2.2 mm;
2.3 keeping the temperature for 6 hours at the temperature of 10 ℃, and enabling lacquer wax crystals to grow to 3.6 mm; (ii) a
2.4, adding perlite into the lacquer seed oil under the temperature environment at the end of the step 2.3, and keeping the temperature and stirring for 80 min;
2.5, performing oil-wax separation on the lacquer seed oil treated in the step 2.4, and separating lacquer wax crystals;
3 ] deodorization and dehydration
And (3) deodorizing and dehydrating the lacquer seed oil obtained by the treatment in the step (2) to obtain the finished product lacquer seed oil.
Through detection, the wax content in the lacquer seed oil is 1.8 percent
Example two
Degumming, deacidification and decolorization
Degumming, deacidifying and decolorizing the crude lacquer seed oil at 80 ℃;
crystal growth dewaxing
Carrying out dewaxing treatment on the lacquer seed oil treated in the step 1:
2.1, reducing the temperature of the lacquer seed oil from 58 ℃ to 32 ℃ within 26 hours, and enabling lacquer wax crystals to grow to be 0.55 mm;
2.2 reducing the temperature of the lacquer seed oil to 11 ℃ within 10 hours, and enabling lacquer wax crystals to grow to 1.2 mm;
2.3, preserving the heat for 5 hours at the temperature of 11 ℃, and enabling lacquer wax crystals to grow to 3 mm; (ii) a
2.4, adding perlite into the lacquer seed oil under the temperature environment at the end of the step 2.3, and keeping the temperature and stirring for 50 min;
2.5, performing oil-wax separation on the lacquer seed oil treated in the step 2.4, and separating lacquer wax crystals;
3 ] deodorization and dehydration
And (3) deodorizing and dehydrating the lacquer seed oil obtained by the treatment in the step (2) to obtain the finished product lacquer seed oil.
Through detection, the wax content in the lacquer seed oil is 1.85 percent
EXAMPLE III
Degumming, deacidification and decolorization
Degumming, deacidifying and decolorizing the crude lacquer seed oil at 90 ℃;
crystal growth dewaxing
Carrying out dewaxing treatment on the lacquer seed oil treated in the step 1:
2.1, reducing the temperature of the lacquer seed oil from 56 ℃ to 38 ℃ within 20 hours, and enabling lacquer wax crystals to grow to 0.3 mm;
2.2 reducing the temperature of the lacquer seed oil to 8 ℃ within 15 hours, and enabling lacquer wax crystals to grow to 2.0 mm;
2.3, preserving the heat for 3 hours at the temperature of 8 ℃, and enabling lacquer wax crystals to grow to be 2.8 mm; (ii) a
2.4, adding perlite into the lacquer seed oil under the temperature environment at the end of the step 2.3, and keeping the temperature and stirring for 60 min;
2.5, performing oil-wax separation on the lacquer seed oil treated in the step 2.4, and separating lacquer wax crystals;
3 ] deodorization and dehydration
And (3) deodorizing and dehydrating the lacquer seed oil obtained by the treatment in the step (2) to obtain the finished product lacquer seed oil.
Through detection, the wax content in the lacquer seed oil is 1.8 percent
Example four
1 ] preparation of crude Lacquer seed oil
1.1, putting the lacquer seed nucleolus in alkaline water with the temperature of 80 ℃ and the pH value of 10, stirring for 40min, removing a wax layer on the surface of the lacquer seed nucleolus, and taking out the lacquer seed nucleolus after stirring;
1.2, placing the lacquer seed nucleolus processed in the step 1.1 in hot water at 90 ℃ for stirring for 20min again, removing the residual wax layer on the surface of the lacquer seed nucleolus, and taking out the lacquer seed nucleolus after stirring;
1.3, drying the lacquer seed kernels processed in the step 1.2 at 70 ℃ for 70min, removing water on the surfaces of the lacquer seed kernels, crushing the lacquer seed kernels to 20 meshes after the water is removed, and pressing the milled lacquer seed kernels into a pancake shape of 3 mm;
1.4, drying the thin-cake-shaped lacquer seed kernels processed in the step 1.3 again for 50min at the temperature of 100 ℃ to reduce the water content of the lacquer seed kernels to be less than 2%;
1.5, squeezing the pancake-shaped lacquer seed kernels processed in the step 1.4 to obtain crude lacquer seed oil;
degumming, deacidification and decolorization
Degumming, deacidifying and decolorizing the crude lacquer seed oil at 75 ℃;
in the process of entering the step 3 in the step 2, naturally cooling the lacquer seed oil to 58 ℃;
3 dewaxing by growing crystals
Carrying out dewaxing treatment on the lacquer seed oil treated in the step 1:
3.1, reducing the temperature of the lacquer seed oil from 52 ℃ to 38 ℃ within 22 hours;
3.2, cooling the lacquer seed oil to 7 ℃ within 12 hours;
3.3, preserving the heat for 5 hours at the temperature of 7 ℃;
3.4, adding a filter aid into the lacquer seed oil at the temperature environment when the step 2.3 is finished, and keeping the temperature and stirring for 65 min;
3.5, performing oil-wax separation on the lacquer seed oil treated in the step 2.4, and filtering the lacquer wax;
4 ] deodorization and dehydration
And (3) deodorizing and dehydrating the lacquer seed oil obtained by the treatment in the step (2) to obtain the finished product lacquer seed oil.
The detection shows that the wax content in the lacquer seed oil is 1.5 percent
EXAMPLE five
1 ] preparation of crude Lacquer seed oil
1.1, putting the lacquer seed nucleolus in alkaline water with the temperature of 90 ℃ and the pH value of 12, stirring for 20min, removing a wax layer on the surface of the lacquer seed nucleolus, and taking out the lacquer seed nucleolus after stirring;
1.2, placing the lacquered seed nucleolus processed in the step 1.1 in hot water at 90 ℃ to stir for 25min again, removing the residual wax layer on the surface of the lacquered seed nucleolus, and taking out the lacquered seed nucleolus after stirring;
1.3, drying the lacquer seed kernels processed in the step 1.2 at 73 ℃ for 68min, removing water on the surfaces of the lacquer seed kernels, crushing the lacquer seed kernels to 40 meshes after the water is removed, and pressing the milled lacquer seed kernels into 2mm thin cakes;
1.4, drying the thin-cake-shaped lacquer seed kernels processed in the step 1.3 again for 70min at 90 ℃ to reduce the water content of the lacquer seed kernels to below 2%;
1.5, squeezing the pancake-shaped lacquer seed kernels processed in the step 1.4 to obtain crude lacquer seed oil;
degumming, deacidification and decolorization
Degumming, deacidifying and decolorizing the crude lacquer seed oil at 83 ℃;
in the process of entering the step 3 in the step 2, naturally cooling the lacquer seed oil to 55 ℃;
3 dewaxing by growing crystals
Carrying out dewaxing treatment on the lacquer seed oil treated in the step 1:
3.1, reducing the temperature of the lacquer seed oil from 54 ℃ to 37 ℃ within 28 hours;
3.2, cooling the lacquer seed oil to 10 ℃ within 6 hours;
3.3, preserving the heat for 4 hours at the temperature of 10 ℃;
3.4, adding a filter aid into the lacquer seed oil at the temperature environment when the step 2.3 is finished, and keeping the temperature and stirring for 70 min;
3.5, performing oil-wax separation on the lacquer seed oil treated in the step 2.4, and filtering the lacquer wax;
4 ] deodorization and dehydration
And (3) deodorizing and dehydrating the lacquer seed oil obtained by the treatment in the step (2) to obtain the finished product lacquer seed oil.
Through detection, the wax content in the lacquer seed oil is 1.75 percent
EXAMPLE six
1 ] preparation of crude Lacquer seed oil
1.1, putting the lacquer seed nucleolus in alkaline water with the temperature of 86 ℃ and the pH value of 11, stirring for 30min, removing a wax layer on the surface of the lacquer seed nucleolus, and taking out the lacquer seed nucleolus after stirring;
1.2, placing the lacquered seed nucleolus processed in the step 1.1 in hot water at 86 ℃ for stirring for 30min again, removing the residual wax layer on the surface of the lacquered seed nucleolus, and taking out the lacquered seed nucleolus after stirring;
1.3, drying the lacquer seed kernels processed in the step 1.2 at 80 ℃ for 70min, removing water on the surfaces of the lacquer seed kernels, crushing the lacquer seed kernels to 30 meshes after the water is removed, and pressing the milled lacquer seed kernels into a 1mm thin cake shape;
1.4, drying the thin-cake-shaped lacquer seed kernels processed in the step 1.3 again for 55min at the temperature of 98 ℃ to reduce the water content of the lacquer seed kernels to be below 2%;
1.5, squeezing the pancake-shaped lacquer seed kernels processed in the step 1.4 to obtain crude lacquer seed oil;
degumming, deacidification and decolorization
Degumming, deacidifying and decolorizing the crude lacquer seed oil at 82 ℃;
in the process of entering the step 3 in the step 2, naturally cooling the lacquer seed oil to 57 ℃;
3 dewaxing by growing crystals
Carrying out dewaxing treatment on the lacquer seed oil treated in the step 1:
3.1, cooling the lacquer seed oil from 53 ℃ to 32 ℃ within 25 hours;
3.2, cooling the lacquer seed oil to 9 ℃ within 8 hours;
3.3, preserving the heat for 5 hours at the temperature of 9 ℃;
3.4, adding a filter aid into the lacquer seed oil at the temperature environment when the step 2.3 is finished, and keeping the temperature and stirring for 60 min;
3.5, performing oil-wax separation on the lacquer seed oil treated in the step 2.4, and filtering the lacquer wax;
4 ] deodorization and dehydration
And (3) deodorizing and dehydrating the lacquer seed oil obtained by the treatment in the step (2) to obtain the finished product lacquer seed oil.
Through detection, the wax content in the lacquer seed oil is 1.6 percent
The two processing schemes can be carried out in a lacquer seed oil processing device:
the lacquer seed oil processing device comprises a rough-making tank 1, a squeezing tank 2, a refining tank 3 and a dewatering tank 4 which are sequentially arranged according to the processing procedure; examples 1 to 3 may be selected to be applicable only to the refining tank 3 and the dewatering tank 4, and examples 4 to 6 may be used in their entirety.
Wherein rough jar 1 is used for carrying out the primary processing to the lacquer seed, and the primary objective of primary processing is to get rid of wax layer and the wax layer residue on seed surface, need spray buck and clear water simultaneously in the course of working, gets rid of respectively, gets rid of and still need dry the lacquer seed after accomplishing, consequently will roughly the jar design as follows structure:
the rough-making tank 1 comprises a rough-making tank body 12 arranged on a rough-making tank support frame 11, a spiral stirrer 13 for stirring paint seeds is arranged in the rough-making tank body 12, a filter screen 14 is arranged below the spiral stirrer 13, an alkali water spray pipe 15 and a clear water spray pipe 16 are arranged at the top of the rough-making tank body 12, and a liquid discharge port 17 is arranged at the bottom of the rough-making tank body 12; the rough tank body 12 is also provided with a first heating unit 18;
when the device is used, firstly, the lacquer seeds are put into the rough tank body 1, the alkaline water spraying pipe 15 is started, alkaline water with the pH value approximately equal to 10 is sprayed for soaking, meanwhile, the spiral stirrer 13 is started, the driving motor is controlled to rotate forwards and backwards for stirring, the first heating unit 18 is started for heating in the stirring process, and the dewaxing efficiency is improved;
after the preliminary operation is finished, a liquid outlet 17 is opened, alkaline water with wax dissolved is discharged through a filter screen 14 and the liquid outlet 17, then the liquid outlet 17 is closed, a clear water spray pipe 16 is opened for spraying and soaking, meanwhile, a spiral stirrer 13 is opened, a driving motor is controlled to rotate forward and backward for stirring, a first heating unit 18 is started for heating in the stirring process, and dewaxing is further carried out;
after the completion, the liquid outlet 17 is opened, the clean water with the wax dissolved therein is discharged through the filter screen 14 and the liquid outlet 17, then the liquid outlet 17 is closed, and simultaneously the spiral stirrer 13 is opened, and the driving motor is controlled to rotate forward and backward to stir and dry;
after the drying is finished, the rough lacquer seeds are discharged through a rough material outlet 19 arranged on the side wall of the rough tank body 12, the lower edge of the outlet of the rough material outlet 19 can be slightly lower than the upper edge of the filter screen 14 and inclined, so that the rough lacquer seeds can be discharged conveniently, and the spiral stirrer 13 is opened during the discharge, so that the rough lacquer seeds can be pushed to move towards the rough material outlet 19.
The discharged crude lacquer seeds are crushed and then sent into a pressing tank 2 to be pressed into a pancake shape of 3mm, and the pancake shape is dried, so that the pressing tank is designed into the following structure:
the pressing tank 2 comprises a pressing tank body 21 and a pressing plate 22, a filtering plate 23 is arranged in the pressing tank body 21, and a second heating unit 24 is arranged at the bottom of the pressing tank body 21. The pressing plates can be selected in many structural modes, and only oil can be extruded from the crushed rough lacquer seeds by simple structure, which is taken as an example in the embodiment, and when the T-shaped pressing plate 22 is installed, the guide plate 26 is arranged at the top of the tank body 21 of the pressing tank; the T-press 22 includes a press plate and a power plate that is adapted to the guide plate 26 and provides power to the power plate in a variety of ways, such as a telescopic cylinder, etc.
When in use, crushed crude lacquer seeds are fed into the pressing tank body 21, the T-shaped pressing plate moves, the pressing plate is pressed with the filter plate 23, the lacquer seed oil flows into the lower part of the filter plate 23 and flows out through a pressing oil outlet 25 arranged on the pressing tank body 21, and for facilitating the outflow, the lower edge of the pressing oil outlet 25 is preferably slightly lower than the upper edge of the second heating unit 24 and is inclined.
After the preliminary completion, the second heating unit 24 is started to dry the thin cake-shaped lacquer seeds until the lacquer seed oil is discharged, so that the water content of the lacquer seeds is lower than 2%, and the oil can be repeatedly squeezed out in the process.
The lacquer seed oil discharged from the pressing tank 2 is sent into the refining tank 3 for degumming, deacidification, decoloration and crystal growth dewaxing treatment, and because the processes of adding water, heating, stirring, oil-wax separation and the like are required in the processes, the refining tank is designed into the following structure:
the refining tank 3 comprises a refining tank body 32 on a refining tank support frame 31, a first stirrer 39 is arranged in the refining tank body 32, the top of the refining tank body 32 is connected with a water inlet pipe 33 and a reagent unit 34, the side wall of the refining tank body 32 is provided with a feed pipe 35, and the bottom of the refining tank body 32 is connected with one end of a discharge pipe 36 and an impurity discharge pipe 37; the refining tank body 32 is also provided with a third heating unit 38; in order to improve the processing precision and the production efficiency, a vacuumizing unit 5, a temperature detection unit 6 and a pressure detection unit 7 can be arranged at the top of the refining tank body 32.
When the device is used, the lacquer seed oil is firstly sent into the refining tank body 32 through the feeding pipe 35, then the first stirrer 39 and the third heating unit 38 are started for heating and stirring, the reagent unit 34 can be started in the process, reactants for degumming, deacidification and decoloration are added for relevant reactions, and finally the substances are discharged through the impurity discharging pipe 37.
Performing crystal growing dewaxing treatment after degumming, deacidification and decoloration, wherein the crystal growing dewaxing process mainly controls the temperature, and only needs to strictly control the third heating unit 38, for example, water with corresponding temperature is introduced into the third heating unit 38 to adjust and control; constantly observe through temperature detecting element 6 and pressure detecting element 7 and adjust, make the wax crystallization that contains in the lacquer seed oil, then open discharging pipe 36 and discharge lacquer seed oil, consider to avoid impurity and crystallization wax to mix into lacquer seed oil and get into next processing link, can set up the high density filter screen at discharging pipe 36.
The high-quality lacquer seed oil obtained by the treatment of the refining tank 3 is finally sent to a dewatering tank 4 for dehydration and deodorization treatment, and refined lacquer seed oil can be obtained after the treatment is finished, so that the dewatering tank is designed into the following structure:
the dehydration tank 4 comprises a dehydration tank body 42 on a dehydration tank support frame 41, a second stirrer 43 is arranged in the dehydration tank body 42, and a fourth heating unit 45 is also arranged on the dehydration tank body 42; the other end of the discharge pipe 36 is connected with a dewatering tank body 42, a discharge pipe 44 is arranged at the bottom of the dewatering tank body 42, and a material receiving unit 8 is arranged below the discharge pipe 44. In order to improve the processing precision and the production efficiency, a vacuumizing unit 5, a temperature detection unit 6 and a pressure detection unit 7 can be arranged at the top of the dewatering tank body 42 in the same way.
The dehydration and deodorization process is mainly temperature control, so that when the refined lacquer seed oil is sent into the dehydration tank body 42, the fourth heating unit 45 and the second stirrer 43 are started for heating and stirring, and finally the refined lacquer seed oil is discharged.
Claims (10)
1. The lacquer seed oil dewaxing process is characterized by comprising the following steps:
degumming, deacidification and decolorization
Degumming, deacidifying and decolorizing the crude lacquer seed oil at 70-90 ℃;
crystal growth dewaxing
Carrying out dewaxing treatment on the lacquer seed oil treated in the step 1):
2.1, slowly reducing the temperature of the lacquer seed oil from 55 +/-3 ℃ to 35 +/-3 ℃ within 20-30 hours, and separating out lacquer wax crystals growing to 0.3-0.7 mm in the temperature reduction process;
2.2, slowly reducing the temperature of the lacquer seed oil from the temperature at the end of the step 2.1 to 8 +/-3 ℃ within 6-15 hours, and continuously precipitating lacquer wax crystals to grow to 1.2-2.2 mm;
2.3, preserving the heat for 3-6 hours in the temperature environment at the end of the step 2.2, and further precipitating lacquer wax crystals to grow to 2.8-3.6 mm; (ii) a
2.4, adding a filter aid accounting for 1.5 to 2.5 percent of the weight of the lacquer seed oil into the lacquer seed oil in the temperature environment at the end of the step 2.3, and stirring for 50 to 80min under heat preservation;
2.5, performing oil-wax separation on the lacquer seed oil treated in the step 2.4, and separating lacquer wax crystals;
3 ] deodorization and dehydration
And (3) deodorizing and dehydrating the lacquer seed oil obtained by the treatment in the step (2) to obtain the finished product lacquer seed oil.
2. The lacquer seed oil dewaxing process of claim 1, wherein: in the step 1, degumming, deacidifying and decoloring are carried out on the crude lacquer seed oil at the temperature of 80 ℃.
3. The lacquer seed oil dewaxing process of claim 2, wherein: in the step 2.1, the temperature of the lacquer seed oil is reduced from 50 ℃ to 35 ℃; in said step 2.2, the temperature is lowered to 10 ℃.
4. The lacquer seed oil dewaxing process of claim 3, wherein: in the step 2.4, the filter aid is perlite.
5. The lacquer seed oil dewaxing process of claim 4, wherein: the slow cooling in the steps 2.1 and 2.2 is realized by adopting a refining tank, the refining tank (3) comprises a refining tank body (32) on a refining tank support frame (31), a first stirrer (39) is arranged in the refining tank body (32), the top of the refining tank body (32) is connected with a water inlet pipe (33) and a reagent unit (34), the side wall of the refining tank body (32) is provided with a feeding pipe (35), and the bottom of the refining tank body (32) is connected with one end of a discharging pipe (36) and an impurity discharging pipe (37); the refining tank body (32) is also provided with a third heating unit (38); the third heating unit (38) is a heating coil wound on the tank body, and liquid is introduced into the heating coil to control the cooling process.
6. The production process of the lacquer seed oil is characterized by comprising the following steps of:
1 ] preparation of crude Lacquer seed oil
1.1, putting the lacquer seed nucleolus in alkaline water with the temperature of 80-90 ℃ and the pH value of 10-12, stirring for 20-40 min, removing a wax layer on the surface of the lacquer seed nucleolus, and taking out the lacquer seed nucleolus after stirring;
1.2, placing the lacquer seed nucleolus processed in the step 1.1 in hot water at the temperature of 80-90 ℃ to be stirred for 20-40 min again, removing the residual wax coat on the surface of the lacquer seed nucleolus, and taking out the lacquer seed nucleolus after stirring;
1.3, drying the lacquer seed kernels treated in the step 1.2 at the temperature of 70-80 ℃ for 50-70 min, removing water on the surfaces of the lacquer seed kernels, crushing the lacquer seed kernels to 20-40 meshes after the water is removed, and pressing the milled lacquer seed kernels into a pancake shape of 1-3 mm;
1.4, drying the thin-cake-shaped lacquer seed kernels processed in the step 1.3 again for 50-70 min at the temperature of 90-100 ℃ to reduce the water content of the lacquer seed kernels to below 2%;
1.5, squeezing the pancake-shaped lacquer seed kernels processed in the step 1.4 to obtain crude lacquer seed oil;
degumming, deacidification and decolorization
Degumming, deacidifying and decolorizing the crude lacquer seed oil at 70-90 ℃;
3 dewaxing by growing crystals
Carrying out dewaxing treatment on the lacquer seed oil treated in the step 1:
3.1, slowly reducing the temperature of the lacquer seed oil from 55 +/-3 ℃ to 35 +/-3 ℃ within 20-30 hours, and separating out lacquer wax crystals growing to 0.3-0.7 mm in the temperature reduction process;
3.2, slowly reducing the temperature of the lacquer seed oil from the temperature at the end of the step 3.1 to 8 +/-3 ℃ within 6-15 hours, and continuously precipitating lacquer wax crystals to grow to 1.2-2.2 mm;
3.3, preserving the heat for 3-6 hours in the temperature environment at the end of the step 3.2, and further precipitating lacquer wax crystals to grow to 2.8-3.6 mm; (ii) a
3.4, adding a filter aid accounting for 1.5 to 2.5 percent of the weight of the lacquer seed oil into the lacquer seed oil in the temperature environment at the end of the step 3.3, and stirring for 50 to 80min under heat preservation;
3.5, performing oil-wax separation on the lacquer seed oil treated in the step 3.4, and separating lacquer wax crystals;
4 ] deodorization and dehydration
And (3) deodorizing and dehydrating the lacquer seed oil obtained by the treatment in the step (2) to obtain the finished product lacquer seed oil.
7. The lacquer seed oil dewaxing process of claim 6, wherein: in the step 2, degumming, deacidifying and decoloring the crude lacquer seed oil at 80 ℃.
8. The lacquer seed oil dewaxing process of claim 7, wherein: in the step 3.1, the temperature of the lacquer seed oil is reduced from 50 ℃ to 35 ℃; in said step 3.2 ], the temperature is lowered to 10 ℃.
9. The lacquer seed oil dewaxing process of claim 8, wherein: in the step 3.4, the filter aid is perlite.
10. The lacquer seed oil dewaxing process of claim 9, wherein: the slow cooling in the steps 3.1 and 3.2 is realized by adopting a refining tank, the refining tank (3) comprises a refining tank body (32) on a refining tank support frame (31), a first stirrer (39) is arranged in the refining tank body (32), the top of the refining tank body (32) is connected with a water inlet pipe (33) and a reagent unit (34), the side wall of the refining tank body (32) is provided with a feeding pipe (35), and the bottom of the refining tank body (32) is connected with one end of a discharging pipe (36) and an impurity discharging pipe (37); the refining tank body (32) is also provided with a third heating unit (38); the third heating unit (38) is a heating coil wound on the tank body, and liquid is introduced into the heating coil to control the cooling process.
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CN102433220A (en) * | 2011-10-31 | 2012-05-02 | 郑州远洋油脂工程技术有限公司 | Oil dewaxing process and device |
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Application publication date: 20210518 |