CN108485530B - Production process and equipment of food-grade rosin - Google Patents
Production process and equipment of food-grade rosin Download PDFInfo
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- CN108485530B CN108485530B CN201810338707.1A CN201810338707A CN108485530B CN 108485530 B CN108485530 B CN 108485530B CN 201810338707 A CN201810338707 A CN 201810338707A CN 108485530 B CN108485530 B CN 108485530B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09F—NATURAL RESINS; FRENCH POLISH; DRYING-OILS; OIL DRYING AGENTS, i.e. SICCATIVES; TURPENTINE
- C09F1/00—Obtaining purification, or chemical modification of natural resins, e.g. oleo-resins
- C09F1/02—Purification
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention relates to the technical field of rosin processing, in particular to a production process and equipment of food-grade rosin. The production process of the food-grade rosin comprises the following steps: A. dissolving; B. coarse settling and separating; C. adding a complexing agent; D. washing with water; E. fine settling, cleaning and separating; F. distilling and preheating; G. vacuum distillation; H. and (5) recovering turpentine. Production equipment of food-grade rosin comprises a dissolving pot (1), a turpentine recycling storage tank (2), a dosing tank (3), a high-level pot (4), a filter (5), a first reaction kettle (6), a second reaction kettle (7), a lifting pump (8), a complexing agent dosing tank (9), a washing pot (10), a hot water pot (11), a fine settling pot (12), a low-level storage tank (13), a distillation pump (14), a preheater (15), a distillation pot (16) and a fragrance releasing tank (17). The invention effectively removes heavy metals, saves energy and water resources, improves the distillation efficiency and reduces the production cost.
Description
Technical Field
The invention relates to the technical field of rosin processing, in particular to a production process and equipment of food-grade rosin.
Background
Gum rosin, which is prepared from rosin, is a transparent, hard and brittle solid with a conchoidal fracture surface and a glass luster, and the color is determined by the quality of the raw materials and the processing technology, and is generally light yellow to reddish brown.
Gum rosin is soluble in a variety of organic solvents, such as: ethanol, ether, acetone, benzene, carbon disulfide, turpentine and the like, but are insoluble in water, the relative density of the materials is 1.05-1.10, and the softening point of the materials is above 74 ℃.
Gum rosin has the property of being easily crystallized, i.e., crystals of resin acids are formed in thick and transparent rosin masses, so that gum rosin becomes cloudy and opaque. The crystalline rosin has a high melting point of 110-135 ℃, is difficult to saponify, and tends to be recrystallized in common organic solvents, so that the use value of the crystalline rosin in industries such as soap, paper making, paint and the like is reduced.
Gum rosin is composed of a variety of resin acids, the chemical nature of which is determined by the various reactions that can be produced by the resin acids. The resin acid molecule has two chemical reaction centers, i.e., a double bond and a carboxyl group. Owing to the double bond reaction and carboxyl reaction of resin acid, rosin is easy to isomerize and has the reaction of addition, disproportionation, polymerization, ammonolysis, esterification, salification, decarboxylation, etc. By utilizing the reactions, the rosin can be modified to prepare a series of modified rosins, so that the use value of the gum rosin is improved. If disproportionation reaction is utilized, disproportionated rosin can be produced; polymerized rosin can be produced by utilizing polymerization reaction; hydrogenated rosin can be produced by hydrogenation reaction; by utilizing the addition reaction, maleated rosin and the like can be produced. The rosin modified products have stable properties and are more widely applied in various industries.
Gum rosin is a mixture of several components, which differ slightly from pine species, and is composed mainly of resin acids with small amounts of fatty acids and neutral substances. According to analysis, in general rosin, the content of resin acid is 85.6-88.7%, the content of fatty acid is 2.5-5.4%, and the content of neutral substance is 5.2-7.6%.
The natural gum rosin is nontoxic, and the harmful components are heavy metal lead, arsenic, organic volatile matters and the like carried in the natural gum rosin. If the harmful metal content such as heavy metal and the organic volatile matters in the natural gum rosin can be removed, the natural gum rosin can be used in the food industry and the medicine industry.
Gum rosin has a long history of direct use in the pharmaceutical and food industries: the main effects are summarized as follows:
(I) Ben Jing: abscess, deep-rooted carbuncle, malignant boil, headache, alopecia, scabies, pruritus and wind-qi, calm the five internal organs and remove heat. ② Biyu (miscellaneous records): it can be used for treating stomach heat, dry throat, diabetes, and wind-arthralgia, and can whiten skin; red blood is mainly manifested as aversion to arthralgia. ③ treatise on herb Property: killing parasites, mainly treating deafness; the teeth have wormholes, and a little bit of the teeth can not be bitten; can be pasted on sores, pustules and bloods, is decocted into paste, promotes tissue regeneration, relieves pain and dispels wind. Fourthly, Rihuazi materia Medica: moistening heart and lung, descending qi and eliminating pathogenic factors; decocted extract is mainly used for fistula and pus discharge. Fifthly, Yunnan Ben Cao: treating red vitiligo and severe wind. Sixthly, the medicine goes to the door: for treating aching pain of the menstrual period, promoting the production of body fluid to quench thirst, strengthening teeth, improving hearing and improving eyesight; when used as a tonic, it can tonify yang and strengthen penis to make one child. Seventh, the compendium: strengthen tendons and bones, benefit ears and eyes, and treat metrorrhagia. Eighty percent (Ben Cao Standby): dispel wind and dampness, remove toxicity and kill parasites.
With the modernization of traditional Chinese medicine and the improvement of living standard of people, the toxic and side effect of the traditional Chinese medicine in the pharmaceutical and food industries is continuously questioned, is mainly influenced by the content of heavy metal and volatile matters in gum rosin, is difficult to remove, and is forbidden to be used in direct oral medicines and direct edible foods. The rosin resin of gum rosin products which are directly used in the pharmaceutical industry and the food industry is food-grade rosin glyceride modified by rosin. However, the modified food-grade rosin glyceride can only be used in the medical adhesive industry and food depilation due to the damaged activity, but not in oral medicines and health care products, and meanwhile, the processing technology is complex, the cost is high, the stability is poor, the quality guarantee period is short (usually only half a year), and the transportation and the use are influenced.
The research and development of the food-grade gum rosin can lead the product to be directly used in the industries of plaster, oral medicine and food, and lead the ancient product to be rejuvenated. The research and development of the food-grade gum rosin are lagged, and no mature product is on the market at home and abroad.
With the development of the medical industry and the improvement of the living standard of people, the health care consciousness of people is gradually improved, the plaster yield of about 18 hundred million plasters is generated in China every year, and famous brands such as large-scale enterprises of Tianhe pharmaceutical industry, LingRui pharmacy, Yunnan white drug powder and the like are provided. Gum rosin is directly used in more than 90 varieties of Chinese medicine quasi-character products with the medicine market capacity of about 3 million tons each year, and is directly listed in the prescription for medicine, such as Renda-Huoluo pill, Foshan ginseng reproduced tablet, Tongluo Huoxue pill, musk hippocampus rheumatalgia-relieving plaster and the like, and is mainly externally used as a main plaster. The food is mainly used as excipient of chewing gum and the like, depilatory of food processing enterprises and the like, and the market capacity is about 5 million tons every year. Because no real food-grade gum rosin exists at present, the product fish dragon used in the market is mixed, some modified rosins such as rosin glyceride with higher use cost are used, and potential harm is brought to physical and mental health of people by using the industrial gum rosin. The national drug administration department stipulates that the raw materials and auxiliary materials used in the medicine need to be used in a medicine grade in the market, and food-grade products are used at least in the market without the medicine grade, and industrial products are strictly forbidden to be used for direct medicine use. The method establishes the regulatory basis for the direct medicine application of the food-grade gum rosin and the market direction, and the food-grade gum rosin has the advantages of cost, stability and other performance indexes compared with the modified rosin, so that the market space is large and the application prospect is very wide.
Disclosure of Invention
The invention provides a production process and equipment of food-grade rosin, which can effectively remove heavy metals, save energy and water resources, improve distillation efficiency and reduce production cost. The production problem of food-grade rosin is effectively solved.
In order to achieve the purpose, the technical solution adopted by the invention is as follows:
the production process of the food-grade rosin comprises the following steps:
A. dissolving: adding turpentine, water and turpentine into a dissolving pot, stirring with steam, heating to dissolve to 90 ℃, and keeping the temperature for 0.5 hour, wherein the mass part ratio of the turpentine to the water to the turpentine is 3: 1: 1, conveying the dissolved rosin mixed solution to a high-level pot by steam pressure through a pipeline;
B. coarse settling and separating: carrying out coarse settling and clear separation on the dissolved rosin mixed solution in an elevated kettle, wherein settling and clear temperature is 85-90 ℃ for 0.5 hour; discharging the lower-layer wastewater after the coarse settling separation from the high-level pot; the upper layer fat liquid is put into a reaction kettle after being coarsely filtered;
C. adding a complexing agent: after the coarse precipitation and separation, feeding the supernatant lipid liquid and the complexing agent into a reaction kettle for stirring for 2 hours, wherein the stirring speed is 30-60 revolutions per minute, and the reaction temperature is 85-90 ℃; the mass ratio of the upper layer fat liquid to the complexing agent is 50: 3; standing for 20 minutes after the reaction is finished, and pumping the complexing agent solution into a solution preparation tank from the bottom for the next use;
D. washing with water: continuously pumping the fat liquid in the reaction kettle into a washing pot, continuously adding hot water, washing in the washing pot at a stirring speed of 30-60 r/min, wherein the mass part ratio of the fat liquid to the hot water is 5: 1, the temperature of hot water is 80-90 ℃; washing the fat liquor and hot water in a water washing pot for 10 minutes; discharging the mixture of the washed fat liquid and the hot water into a fine precipitation pot;
E. fine sediment separation: carrying out fine precipitation separation on the mixture of the washed fat liquid and the hot water in a fine precipitation pot for 8-12 hours, wherein the precipitation temperature is 85-90 ℃, and discharging the lower-layer wastewater after the fine precipitation separation from the fine precipitation pot;
F. distillation preheating: continuously pumping the settled rosin into a preheater to preheat to 140 ℃ and then discharging into a distillation boiler;
G. vacuum distillation: putting the preheated rosin into a distillation kettle for vacuum distillation for 30-40 minutes; the vacuum degree is-0.07-0.08 MPa, and the distillation temperature is 165 ℃; the product left in the distillation kettle after distillation is food-grade rosin;
H. and (3) turpentine recovery: vacuumizing the fine desilting pot and the distilling pot; condensing the extracted gas at vacuum degree of-0.07-0.08 MPa, separating oil from water, dissolving part of the separated oil in turpentine tank, and storing the rest in turpentine tank.
The complexing agent is an aqueous solution of EDTA, potassium citrate, sodium potassium tartrate and ammonium fluoride, and the concentration of the aqueous solution is 0.02-0.03 mol/L.
Production equipment of food-grade rosin comprises a dissolving pot, a turpentine recycling storage tank, a batching tank, a high-level pot, a filter, a first reaction kettle, a second reaction kettle, a lift pump, a complexing agent batching tank, a washing pot, a hot water pot, a fine settling pot, a low-level storage tank, a distillation pump, a preheater, a distillation pot, a fragrance releasing tank, a condenser, an oil-water receiver, a vacuum buffer tank, a vacuum pump, an oil-water separator, a turpentine storage tank and a turpentine oil recovery pump;
the turpentine inlet oil port of the dissolving pot is connected with the oil outlet of the turpentine recycling storage tank through a pipeline, and a turpentine liquid inlet valve is arranged on the pipeline; the feed port of the dissolving pot is connected with the batching tank through a pipeline, and a feed valve is arranged on the pipeline; the water inlet of the dissolving pot is connected through a tap water pipe, and a water inlet valve of the dissolving pot is arranged on the tap water pipe; the liquid outlet of the dissolving pot is connected with the feed inlet of the high-level pot through a material pipeline, and a material valve is arranged on the material pipe; a steam pipeline is arranged on the dissolving pot, and a steam inlet valve is arranged on the steam pipeline;
the high-level pot discharging port is connected with the liquid inlet of the filter through a pipeline, and a high-level pot discharging valve is arranged on the pipeline; the lower part of the high-level pot is provided with a high-level pot blow-off pipe which is provided with a high-level pot blow-off valve;
the liquid outlet of the filter is respectively connected with the grease inlets of the first reaction kettle and the second reaction kettle through pipelines, and the pipelines are provided with a grease inlet valve of the first reaction kettle and a grease inlet valve of the second reaction kettle; the bottom of the reaction kettle is connected with a liquid inlet of the lift pump through a pipeline, and a first reaction kettle liquid discharge valve and a second reaction kettle liquid discharge valve are respectively arranged on the pipeline;
the liquid outlet of the lifting pump is connected with the liquid inlet of the complexing agent liquid preparation tank and the grease inlet of the water washing pot through pipelines, and the pipelines are respectively provided with a complexing agent liquid return valve and a grease inlet valve of the water washing pot; a liquid outlet of the complexing agent preparation tank is connected with complexing agent inlet ports of the first reaction kettle and the second reaction kettle through pipelines, and a complexing agent inlet valve of the first reaction kettle and a complexing agent inlet valve of the second reaction kettle are respectively arranged on the pipelines;
the water outlet of the hot water pot is connected with the water inlet of the water washing pot through a hot water inlet pipe, and a hot water inlet valve of the water washing pot is arranged on the hot water inlet pipe; the liquid outlet of the washing pot is connected with the liquid inlet of the fine precipitation pot through a pipeline, and a liquid outlet valve of the washing pot is arranged on the pipeline;
the fine settling pan fat outlet is connected with the low-level storage tank fat inlet through a pipeline, the fine settling pan is provided with a fine settling pan blow-off pipe, and a fine settling pan blow-off valve is arranged on the fine settling pan blow-off pipe; the liquid outlet of the low-level storage tank is connected with the liquid inlet of the distillation pump through a pipeline, and the liquid outlet of the distillation pump is connected with the grease inlet of the preheater through a pipeline; a vacuum port above the fine desilting pot is connected with a steam inlet of the condenser through a pipeline, and a vacuum valve is arranged on the pipeline;
the grease outlet of the preheater is connected with the feed inlet of the distillation still through a pipeline; the turpentine distillation outlet of the distillation pot is connected with the steam inlet of the condenser through a pipeline; a rosin outlet at the bottom of the distillation pot is connected with the fragrance releasing groove through a pipeline, and a fragrance releasing valve is arranged on the pipeline;
the steam outlet of the condenser is connected with the feed inlet of the oil-water receiver through a pipeline, and the vacuum port of the oil-water receiver is connected with the vacuum buffer tank through a pipeline; the air outlet pipe of the vacuum buffer tank is connected with the air pumping port of the vacuum pump through a vacuum pipe; the discharge port of the oil-water receiver is connected with an oil-water separator through a pipeline, the pipeline is provided with an oil-water receiver discharge valve, and the oil outlet of the oil-water separator is connected with the oil inlet of the turpentine storage tank through a pipeline; an oil outlet of the turpentine storage tank is connected with an oil inlet of a turpentine recycling pump through a pipeline, and an oil outlet of the turpentine recycling pump is connected with an oil inlet of a turpentine recycling storage tank through a pipeline.
When the device works, turpentine, tap water and turpentine in a turpentine recycling storage tank are added into a dissolving pot, stirred by steam and heated to 90 ℃, and the turpentine, the tap water and the turpentine are mixed according to the mass part ratio of 3: 1: 1; the dissolved fat liquid is pumped to a high-level pot by steam. Standing the fat liquid in an elevated kettle for 0.5 hour for coarse separation, and discharging waste water and waste residues from the bottom; discharging the lipid liquid from the discharge port to a filter for filtration. Putting the fat liquid after coarse filtration into a first reaction kettle or a second reaction kettle, adding a complexing agent solution into the reaction kettle, and stirring for 2 hours at the stirring speed of 30-60 revolutions per minute and the reaction temperature of 85-90 ℃; then standing for 20 minutes, after separating the lipid liquid and the complexing liquid, opening a drain valve of a first reaction kettle or a drain valve of a second reaction kettle, opening a complexing agent return valve, and pumping the complexing liquid into a complexing agent preparation tank from the bottom by using a lift pump; when the fat liquid is seen from the bottom view mirror, the complexing agent liquid return valve is closed, the fat liquid inlet valve of the washing pot is opened, the fat liquid is pumped into the washing pot, and meanwhile, hot water is opened for continuous washing operation for 10 minutes. Discharging the mixture of the washed fat liquid and the hot water into a fine precipitation pot for precipitation, and discharging the lower-layer wastewater after the fine precipitation separation from the fine precipitation pot. Putting the settled rosin into a low-level storage tank, pumping the rosin into a preheater by a distillation pump, and preheating to 140 ℃. Putting the preheated rosin into a distillation kettle for vacuum distillation; the vacuum degree is-0.07-0.08 MPa, and the distillation temperature is 165 ℃; the product remaining in the still after distillation is a food grade rosin. Vacuumizing the fine desilting pot and the distilling pot; condensing the extracted gas at a vacuum degree of-0.07 MPa to-0.08 MPa, performing oil-water separation after condensation, storing the separated oil as turpentine in a turpentine storage tank, and pumping part of the turpentine into a turpentine recycling storage tank for a dissolving process.
The invention has the beneficial effects that:
1. the invention effectively removes heavy metals, saves energy and water resources, improves the distillation efficiency and reduces the production cost.
2. The invention adopts the complexing agent to react with heavy metal in the natural gum rosin to form a complex for sedimentation, thereby realizing the separation.
3. The complex reaction is carried out in a reaction kettle, and an intermittent reaction is adopted, so that the reaction is fully carried out, and the reaction is controllable.
4. The invention adopts vacuum distillation, reduces the distillation temperature from 185 ℃ to 165 ℃, reduces the steam consumption, simultaneously reduces the cooling water consumption, and saves energy and water resources; the distillation time is shortened, and the distillation efficiency is improved; the content of organic volatile matters is greatly reduced, so that the distilled rosin meets the quality requirement; the rosin has low fragrance releasing temperature, short high-temperature oxidation isomerization time of more than 150 ℃, lighter color, improved production safety and reduced production cost.
5. The food-grade rosin produced by the invention has the arsenic content of less than or equal to 0.0002, the heavy metal (calculated by Pb) content of less than or equal to 0.001 and the ash content of less than or equal to 0.008, and organic volatile matters are removed.
6. The invention adopts the horn-shaped distributor and the zigzag collector to separate the fat liquid in the settling pan from fine impurities, gravels, wastewater and barks, the flow rate of the fat liquid is greatly reduced after passing through the horn-shaped distributor, the fat liquid slowly moves upwards from the periphery of the horn mouth uniformly under the action of the horn-shaped distributor and the zigzag collector, heavier impurities and wastewater settle downwards under the action of gravity, and the settled fat liquid flows out of the zigzag collector, thereby ensuring good settling effect.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Fig. 2 is a schematic structural diagram of production equipment of the food-grade rosin.
1-dissolving pot, 2-turpentine recycling storage tank, 3-batching tank, 4-high-position pot, 5-filter, 6-first reaction kettle, 7-second reaction kettle, 8-lift pump, 9-complexing agent batching tank, 10-washing pot, 11-hot water pot, 12-fine settling pot, 13-low-position storage tank, 14-distillation pump, 15-preheater, 16-distillation pot, 17-fragrance releasing tank, 18-condenser, 19-oil water receiver, 20-vacuum buffer tank, 21-vacuum pump, 22-oil water separator, 23-turpentine storage tank, 24-turpentine oil recovery pump, 25-turpentine oil inlet valve, 26-feeding valve, 27-dissolving pot water inlet valve, 28-material valve, 29-steam pipeline, 30-steam inlet valve, 31-high-level pot discharge valve, 32-high-level pot drain pipe, 33-high-level pot drain valve, 34-first reaction kettle fat liquid inlet valve, 35-second reaction kettle fat liquid inlet valve, 36-first reaction kettle liquid outlet valve, 37-second reaction kettle liquid outlet valve, 38-complexing agent return valve, 39-washing pot fat liquid inlet valve, 40-first reaction kettle complexing agent inlet valve, 41-second reaction kettle complexing agent inlet valve, 42-washing pot hot water inlet valve, 43-washing pot liquid outlet valve, 44-fine settling pot drain pipe, 45-fine settling pot drain valve, 46-vacuum valve, 47-fragrance discharging valve and 48-oil water receiver discharge valve.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1
As shown in fig. 1 and 2, the production process of the food-grade rosin comprises the following steps:
A. dissolving: adding turpentine, water and turpentine into a dissolving pot, stirring with steam, heating to dissolve to 90 ℃, and keeping the temperature for 0.5 hour, wherein the mass part ratio of the turpentine to the water to the turpentine is 3: 1: 1, conveying the dissolved rosin mixed solution to a high-level pot by steam pressure through a pipeline;
B. coarse settling and separating: carrying out coarse settling and clear separation on the dissolved rosin mixed solution in an elevated kettle, wherein settling and clear temperature is 85-90 ℃ for 0.5 hour; discharging the lower-layer wastewater after the coarse settling separation from the high-level pot; the upper layer fat liquid is put into a reaction kettle after being coarsely filtered;
C. adding a complexing agent: after the coarse precipitation and separation, feeding the supernatant lipid liquid and the complexing agent into a reaction kettle for stirring for 2 hours, wherein the stirring speed is 30 revolutions per minute, and the reaction temperature is 85-90 ℃; the mass ratio of the upper layer fat liquid to the complexing agent is 50: 3; standing for 20 minutes after the reaction is finished, and pumping the complexing agent solution into a solution preparation tank from the bottom for the next use;
D. washing with water: continuously pumping the fat liquid in the reaction kettle into a washing pot, continuously adding hot water, washing in the washing pot at a stirring speed of 30 revolutions per minute, wherein the mass part ratio of the fat liquid to the hot water is 5: 1, the temperature of hot water is 80-90 ℃; washing the fat liquor and hot water in a water washing pot for 10 minutes; discharging the mixture of the washed fat liquid and the hot water into a fine precipitation pot;
E. fine sediment separation: carrying out fine precipitation separation on the mixture of the washed fat liquid and the hot water in a fine precipitation pot for 8 hours, wherein the precipitation temperature is 85-90 ℃, and discharging the lower-layer wastewater after the fine precipitation separation from the fine precipitation pot;
F. distillation preheating: continuously pumping the settled rosin into a preheater to preheat to 140 ℃ and then discharging into a distillation boiler;
G. vacuum distillation: putting the preheated rosin into a distillation kettle for vacuum distillation for 30 minutes; the vacuum degree is-0.07-0.08 MPa, and the distillation temperature is 165 ℃; the product left in the distillation kettle after distillation is food-grade rosin;
H. and (3) turpentine recovery: vacuumizing the fine desilting pot and the distilling pot; condensing the extracted gas at vacuum degree of-0.07-0.08 MPa, separating oil from water, dissolving part of the separated oil in turpentine tank, and storing the rest in turpentine tank.
The complexing agent is an EDTA aqueous solution, and the concentration of the aqueous solution is 0.02 mol/L.
Production equipment of food-grade rosin comprises a dissolving pot 1, a turpentine recycling storage tank 2, a dosing tank 3, a high-level pot 4, a filter 5, a first reaction kettle 6, a second reaction kettle 7, a lifting pump 8, a complexing agent dosing tank 9, a washing pot 10, a hot water pot 11, a fine settling pan 12, a low-level storage tank 13, a distillation pump 14, a preheater 15, a distillation pot 16, a fragrance releasing tank 17, a condenser 18, an oil-water receiver 19, a vacuum buffer tank 20, a vacuum pump 21, an oil-water separator 22, a turpentine storage tank 23 and a turpentine recycling pump 24;
the turpentine inlet oil port of the dissolving pot 1 is connected with the oil outlet of the turpentine recycling storage tank 2 through a pipeline, and a turpentine liquid inlet valve 25 is arranged on the pipeline; the feed port of the dissolving pot 1 is connected with the batching tank 3 through a pipeline, and a feed valve 26 is arranged on the pipeline; the water inlet of the dissolving pot 1 is connected through a tap water pipe, and a water inlet valve 27 of the dissolving pot is arranged on the tap water pipe; the liquid outlet of the dissolving pot 1 is connected with the feed inlet of the high-level pot 4 through a material pipeline, and a material valve 28 is arranged on the material pipeline; a steam pipeline 29 is arranged on the dissolving pot 1, and a steam inlet valve 30 is arranged on the steam pipeline 29;
a discharge port of the high-level pot 4 is connected with a liquid inlet of the filter 5 through a pipeline, and a discharge valve 31 of the high-level pot is arranged on the pipeline; the lower part of the high-level pot 4 is provided with a high-level pot sewage discharge pipe 32, and the high-level pot sewage discharge pipe 32 is provided with a high-level pot sewage discharge valve 33;
a liquid outlet of the filter 5 is respectively connected with a grease inlet of the first reaction kettle 6 and a grease inlet of the second reaction kettle 7 through pipelines, and the pipelines are provided with a grease inlet valve 34 of the first reaction kettle and a grease inlet valve 35 of the second reaction kettle; the bottom of the reaction kettle is connected with a liquid inlet of the lift pump 8 through a pipeline, and a first reaction kettle liquid discharge valve 36 and a second reaction kettle liquid discharge valve 37 are respectively arranged on the pipeline;
a liquid outlet of the lift pump 8 is connected with a liquid inlet of the complexing agent liquid preparation tank 9 and a fat liquid inlet of the water washing pot 10 through pipelines, and a complexing agent liquid return valve 38 and a fat liquid inlet valve 39 of the water washing pot are respectively arranged on the pipelines; a liquid outlet of the complexing agent preparation tank 9 is connected with complexing agent inlets of the first reaction kettle 6 and the second reaction kettle 7 through pipelines, and a first reaction kettle complexing agent feeding valve 40 and a second reaction kettle complexing agent feeding valve 41 are respectively arranged on the pipelines;
the water outlet of the hot water pot 11 is connected with the water inlet of the water washing pot 10 through a hot water inlet pipe, and a hot water inlet valve 42 of the water washing pot is arranged on the hot water inlet pipe; a liquid outlet of the washing pot 10 is connected with a liquid inlet of the fine sedimentation pot 12 through a pipeline, and a liquid outlet valve 43 of the washing pot is arranged on the pipeline;
the outlet of the fine desilting pan 12 is connected with the inlet of the low-level storage tank 13 through a pipeline, the fine desilting pan 12 is provided with a drain pipe 44 of the fine desilting pan, and a drain valve 45 of the fine desilting pan is arranged on the drain pipe 44 of the fine desilting pan; a liquid outlet of the low storage tank 13 is connected with a liquid inlet of a distillation pump 14 through a pipeline, and a liquid outlet of the distillation pump 14 is connected with a grease inlet of a preheater 15 through a pipeline; the vacuum port above the fine precipitation pot 12 is connected with the steam inlet of the condenser 18 through a pipeline, and a vacuum valve 46 is arranged on the pipeline;
a grease outlet of the preheater 15 is connected with a feed inlet of the distillation pot 16 through a pipeline; a turpentine distillation outlet of the distillation pot 16 is connected with a steam inlet of a condenser 18 through a pipeline; a rosin outlet at the bottom of the distillation pot 16 is connected with the fragrance releasing groove 17 through a pipeline, and a fragrance releasing valve 47 is arranged on the pipeline;
a steam outlet of the condenser 18 is connected with a feed inlet of an oil-water receiver 19 through a pipeline, and a vacuum port of the oil-water receiver 19 is connected with a vacuum buffer tank 20 through a pipeline; an air outlet pipe of the vacuum buffer tank 20 is connected with an air suction port of a vacuum pump 21 through a vacuum pipe; the discharge hole of the oil-water receiver 19 is connected with the oil-water separator 22 through a pipeline, an oil-water receiver discharge valve 48 is arranged on the pipeline, and the oil outlet of the oil-water separator 22 is connected with the oil inlet of the turpentine storage tank 23 through a pipeline; an oil outlet of the turpentine storage tank 23 is connected with an oil inlet of a turpentine recycling pump 24 through a pipeline, and an oil outlet of the turpentine recycling pump 24 is connected with an oil inlet of the turpentine recycling storage tank 2 through a pipeline.
When the device works, turpentine in the turpentine recycling storage tank 2, tap water and turpentine is added into the dissolving pot 1, stirred by steam and heated to 90 ℃, and the turpentine, the tap water and the turpentine are mixed according to the mass part ratio of 3: 1: 1; the dissolved fat liquid is pumped to the high-level pot 4 by steam. Standing the fat liquid in an elevated kettle 4 for 0.5 hour for coarse separation, and discharging waste water and waste residues from the bottom; the fat liquid is discharged from the discharge port to the filter 5 for filtration. Putting the fat liquid after coarse filtration into a first reaction kettle or a second reaction kettle, adding a complexing agent solution into the reaction kettle, and stirring for 2 hours at the stirring speed of 30 revolutions per minute and the reaction temperature of 85-90 ℃; then standing for 20 minutes, after separating the lipid liquid and the complexing liquid, opening a first reaction kettle drain valve 36 or a second reaction kettle drain valve 37, opening a complexing agent return valve 38, and pumping the complexing liquid into a complexing agent preparation tank 9 from the bottom by using a lift pump 8; when the fat liquid is seen from the bottom view mirror, the complexing agent liquid return valve 38 is closed, the fat liquid inlet valve 39 of the water washing pot is opened, the fat liquid is pumped into the water washing pot 10, and meanwhile, hot water is opened for continuous water washing operation for 10 minutes. Discharging the mixture of the washed fat liquid and the hot water into a fine precipitation pot 12 for precipitation, and discharging the lower-layer wastewater after the fine precipitation separation from the fine precipitation pot 12. Putting the settled rosin into a low-level storage tank 13, pumping into a preheater 15 by a distillation pump 14, and preheating to 140 ℃. Putting the preheated rosin into a distillation pot 16 for vacuum distillation; the vacuum degree is-0.07-0.08 MPa, and the distillation temperature is 165 ℃; the product remaining in the still 16 after distillation is a food grade rosin. Vacuumizing the fine desilting pot 12 and the distilling pot 16; the vacuum degree is-0.07-0.08 MPa, the extracted gas is condensed, oil-water separation is carried out after condensation, the separated oil is turpentine oil which is stored in a turpentine oil storage tank 23, and part of the turpentine oil is pumped into a turpentine oil recycling storage tank 2 for a dissolving process.
Example 2
The production process of the food-grade rosin comprises the following steps:
A. dissolving: adding turpentine, water and turpentine into a dissolving pot, stirring with steam, heating to dissolve to 90 ℃, and keeping the temperature for 0.5 hour, wherein the mass part ratio of the turpentine to the water to the turpentine is 3: 1: 1, conveying the dissolved rosin mixed solution to a high-level pot by steam pressure through a pipeline;
B. coarse settling and separating: carrying out coarse settling and clear separation on the dissolved rosin mixed solution in an elevated kettle, wherein settling and clear temperature is 85-90 ℃ for 0.5 hour; discharging the lower-layer wastewater after the coarse settling separation from the high-level pot; the upper layer fat liquid is put into a reaction kettle after being coarsely filtered;
C. adding a complexing agent: after the coarse precipitation and separation, feeding the supernatant lipid liquid and the complexing agent into a reaction kettle for stirring for 2 hours, wherein the stirring speed is 45 revolutions per minute, and the reaction temperature is 85-90 ℃; the mass ratio of the upper layer fat liquid to the complexing agent is 50: 3; standing for 20 minutes after the reaction is finished, and pumping the complexing agent solution into a solution preparation tank from the bottom for the next use;
D. washing with water: continuously pumping the fat liquid in the reaction kettle into a washing pot, continuously adding hot water, washing in the washing pot at a stirring speed of 45 revolutions per minute, wherein the mass part ratio of the fat liquid to the hot water is 5: 1, the temperature of hot water is 80-90 ℃; washing the fat liquor and hot water in a water washing pot for 10 minutes; discharging the mixture of the washed fat liquid and the hot water into a fine precipitation pot;
E. fine sediment separation: carrying out fine settling separation on the mixture of the washed fat liquid and the hot water in a fine settling pan for 10 hours at the settling temperature of 85-90 ℃, and discharging lower-layer wastewater after the fine settling separation from the fine settling pan;
F. distillation preheating: continuously pumping the settled rosin into a preheater to preheat to 140 ℃ and then discharging into a distillation boiler;
G. vacuum distillation: putting the preheated rosin into a distillation kettle for vacuum distillation for 35 minutes; the vacuum degree is-0.07-0.08 MPa, and the distillation temperature is 165 ℃; the product left in the distillation kettle after distillation is food-grade rosin;
H. and (3) turpentine recovery: vacuumizing the fine desilting pot and the distilling pot; condensing the extracted gas at vacuum degree of-0.07-0.08 MPa, separating oil from water, dissolving part of the separated oil in turpentine tank, and storing the rest in turpentine tank.
The complexing agent is a potassium citrate aqueous solution, and the concentration of the aqueous solution is 0.025 mol/L.
Production equipment of food-grade rosin comprises a dissolving pot, a turpentine recycling storage tank, a batching tank, a high-level pot, a filter, a first reaction kettle, a second reaction kettle, a lift pump, a complexing agent batching tank, a washing pot, a hot water pot, a fine settling pot, a low-level storage tank, a distillation pump, a preheater, a distillation pot, a fragrance releasing tank, a condenser, an oil-water receiver, a vacuum buffer tank, a vacuum pump, an oil-water separator, a turpentine storage tank and a turpentine oil recovery pump;
the turpentine inlet oil port of the dissolving pot is connected with the oil outlet of the turpentine recycling storage tank through a pipeline, and a turpentine liquid inlet valve is arranged on the pipeline; the feed port of the dissolving pot is connected with the batching tank through a pipeline, and a feed valve is arranged on the pipeline; the water inlet of the dissolving pot is connected through a tap water pipe, and a water inlet valve of the dissolving pot is arranged on the tap water pipe; the liquid outlet of the dissolving pot is connected with the feed inlet of the high-level pot through a material pipeline, and a material valve is arranged on the material pipe; a steam pipeline is arranged on the dissolving pot, and a steam inlet valve is arranged on the steam pipeline;
the high-level pot discharging port is connected with the liquid inlet of the filter through a pipeline, and a high-level pot discharging valve is arranged on the pipeline; the lower part of the high-level pot is provided with a high-level pot blow-off pipe which is provided with a high-level pot blow-off valve;
the liquid outlet of the filter is respectively connected with the grease inlets of the first reaction kettle and the second reaction kettle through pipelines, and the pipelines are provided with a grease inlet valve of the first reaction kettle and a grease inlet valve of the second reaction kettle; the bottom of the reaction kettle is connected with a liquid inlet of the lift pump through a pipeline, and a first reaction kettle liquid discharge valve and a second reaction kettle liquid discharge valve are respectively arranged on the pipeline;
the liquid outlet of the lifting pump is connected with the liquid inlet of the complexing agent liquid preparation tank and the grease inlet of the water washing pot through pipelines, and the pipelines are respectively provided with a complexing agent liquid return valve and a grease inlet valve of the water washing pot; a liquid outlet of the complexing agent preparation tank is connected with complexing agent inlet ports of the first reaction kettle and the second reaction kettle through pipelines, and a complexing agent inlet valve of the first reaction kettle and a complexing agent inlet valve of the second reaction kettle are respectively arranged on the pipelines;
the water outlet of the hot water pot is connected with the water inlet of the water washing pot through a hot water inlet pipe, and a hot water inlet valve of the water washing pot is arranged on the hot water inlet pipe; the liquid outlet of the washing pot is connected with the liquid inlet of the fine precipitation pot through a pipeline, and a liquid outlet valve of the washing pot is arranged on the pipeline;
the fine settling pan fat outlet is connected with the low-level storage tank fat inlet through a pipeline, the fine settling pan is provided with a fine settling pan blow-off pipe, and a fine settling pan blow-off valve is arranged on the fine settling pan blow-off pipe; the liquid outlet of the low-level storage tank is connected with the liquid inlet of the distillation pump through a pipeline, and the liquid outlet of the distillation pump is connected with the grease inlet of the preheater through a pipeline; a vacuum port above the fine desilting pot is connected with a steam inlet of the condenser through a pipeline, and a vacuum valve is arranged on the pipeline;
the grease outlet of the preheater is connected with the feed inlet of the distillation still through a pipeline; the turpentine distillation outlet of the distillation pot is connected with the steam inlet of the condenser through a pipeline; a rosin outlet at the bottom of the distillation pot is connected with the fragrance releasing groove through a pipeline, and a fragrance releasing valve is arranged on the pipeline;
the steam outlet of the condenser is connected with the feed inlet of the oil-water receiver through a pipeline, and the vacuum port of the oil-water receiver is connected with the vacuum buffer tank through a pipeline; the air outlet pipe of the vacuum buffer tank is connected with the air pumping port of the vacuum pump through a vacuum pipe; the discharge port of the oil-water receiver is connected with an oil-water separator through a pipeline, the pipeline is provided with an oil-water receiver discharge valve, and the oil outlet of the oil-water separator is connected with the oil inlet of the turpentine storage tank through a pipeline; an oil outlet of the turpentine storage tank is connected with an oil inlet of a turpentine recycling pump through a pipeline, and an oil outlet of the turpentine recycling pump is connected with an oil inlet of a turpentine recycling storage tank through a pipeline.
When the device works, turpentine, tap water and turpentine in a turpentine recycling storage tank are added into a dissolving pot, stirred by steam and heated to 90 ℃, and the turpentine, the tap water and the turpentine are mixed according to the mass part ratio of 3: 1: 1; the dissolved fat liquid is pumped to a high-level pot by steam. Standing the fat liquid in an elevated kettle for 0.5 hour for coarse separation, and discharging waste water and waste residues from the bottom; discharging the lipid liquid from the discharge port to a filter for filtration. Putting the fat liquid after coarse filtration into a first reaction kettle or a second reaction kettle, adding a complexing agent solution into the reaction kettle, and stirring for 2 hours at the stirring speed of 45 revolutions per minute and the reaction temperature of 85-90 ℃; then standing for 20 minutes, after separating the lipid liquid and the complexing liquid, opening a drain valve of a first reaction kettle or a drain valve of a second reaction kettle, opening a complexing agent return valve, and pumping the complexing liquid into a complexing agent preparation tank from the bottom by using a lift pump; when the fat liquid is seen from the bottom view mirror, the complexing agent liquid return valve is closed, the fat liquid inlet valve of the washing pot is opened, the fat liquid is pumped into the washing pot, and meanwhile, hot water is opened for continuous washing operation for 10 minutes. Discharging the mixture of the washed fat liquid and the hot water into a fine precipitation pot for precipitation, and discharging the lower-layer wastewater after the fine precipitation separation from the fine precipitation pot. Putting the settled rosin into a low-level storage tank, pumping the rosin into a preheater by a distillation pump, and preheating to 140 ℃. Putting the preheated rosin into a distillation kettle for vacuum distillation; the vacuum degree is-0.07-0.08 MPa, and the distillation temperature is 165 ℃; the product remaining in the still after distillation is a food grade rosin. Vacuumizing the fine desilting pot and the distilling pot; condensing the extracted gas at a vacuum degree of-0.07 MPa to-0.08 MPa, performing oil-water separation after condensation, storing the separated oil as turpentine in a turpentine storage tank, and pumping part of the turpentine into a turpentine recycling storage tank for a dissolving process.
Example 3
The production process of the food-grade rosin comprises the following steps:
A. dissolving: adding turpentine, water and turpentine into a dissolving pot, stirring with steam, heating to dissolve to 90 ℃, and keeping the temperature for 0.5 hour, wherein the mass part ratio of the turpentine to the water to the turpentine is 3: 1: 1, conveying the dissolved rosin mixed solution to a high-level pot by steam pressure through a pipeline;
B. coarse settling and separating: carrying out coarse settling and clear separation on the dissolved rosin mixed solution in an elevated kettle, wherein settling and clear temperature is 85-90 ℃ for 0.5 hour; discharging the lower-layer wastewater after the coarse settling separation from the high-level pot; the upper layer fat liquid is put into a reaction kettle after being coarsely filtered;
C. adding a complexing agent: after the coarse precipitation and separation, feeding the supernatant lipid liquid and the complexing agent into a reaction kettle for stirring for 2 hours, wherein the stirring speed is 45 revolutions per minute, and the reaction temperature is 85-90 ℃; the mass ratio of the upper layer fat liquid to the complexing agent is 50: 3; standing for 20 minutes after the reaction is finished, and pumping the complexing agent solution into a solution preparation tank from the bottom for the next use;
D. washing with water: continuously pumping the fat liquid in the reaction kettle into a washing pot, continuously adding hot water, washing in the washing pot at a stirring speed of 45 revolutions per minute, wherein the mass part ratio of the fat liquid to the hot water is 5: 1, the temperature of hot water is 80-90 ℃; washing the fat liquor and hot water in a water washing pot for 10 minutes; discharging the mixture of the washed fat liquid and the hot water into a fine precipitation pot;
E. fine sediment separation: carrying out fine settling separation on the mixture of the washed fat liquid and the hot water in a fine settling pan for 10 hours at the settling temperature of 85-90 ℃, and discharging lower-layer wastewater after the fine settling separation from the fine settling pan;
F. distillation preheating: continuously pumping the settled rosin into a preheater to preheat to 140 ℃ and then discharging into a distillation boiler;
G. vacuum distillation: putting the preheated rosin into a distillation kettle for vacuum distillation for 35 minutes; the vacuum degree is-0.07-0.08 MPa, and the distillation temperature is 165 ℃; the product left in the distillation kettle after distillation is food-grade rosin;
H. and (3) turpentine recovery: vacuumizing the fine desilting pot and the distilling pot; condensing the extracted gas at vacuum degree of-0.07-0.08 MPa, separating oil from water, dissolving part of the separated oil in turpentine tank, and storing the rest in turpentine tank.
The complexing agent is an aqueous solution of potassium sodium tartrate, and the concentration of the aqueous solution is 0.025 mol/L.
Production equipment of food-grade rosin comprises a dissolving pot, a turpentine recycling storage tank, a batching tank, a high-level pot, a filter, a first reaction kettle, a second reaction kettle, a lift pump, a complexing agent batching tank, a washing pot, a hot water pot, a fine settling pot, a low-level storage tank, a distillation pump, a preheater, a distillation pot, a fragrance releasing tank, a condenser, an oil-water receiver, a vacuum buffer tank, a vacuum pump, an oil-water separator, a turpentine storage tank and a turpentine oil recovery pump;
the turpentine inlet oil port of the dissolving pot is connected with the oil outlet of the turpentine recycling storage tank through a pipeline, and a turpentine liquid inlet valve is arranged on the pipeline; the feed port of the dissolving pot is connected with the batching tank through a pipeline, and a feed valve is arranged on the pipeline; the water inlet of the dissolving pot is connected through a tap water pipe, and a water inlet valve of the dissolving pot is arranged on the tap water pipe; the liquid outlet of the dissolving pot is connected with the feed inlet of the high-level pot through a material pipeline, and a material valve is arranged on the material pipe; a steam pipeline is arranged on the dissolving pot, and a steam inlet valve is arranged on the steam pipeline;
the high-level pot discharging port is connected with the liquid inlet of the filter through a pipeline, and a high-level pot discharging valve is arranged on the pipeline; the lower part of the high-level pot is provided with a high-level pot blow-off pipe which is provided with a high-level pot blow-off valve;
the liquid outlet of the filter is respectively connected with the grease inlets of the first reaction kettle and the second reaction kettle through pipelines, and the pipelines are provided with a grease inlet valve of the first reaction kettle and a grease inlet valve of the second reaction kettle; the bottom of the reaction kettle is connected with a liquid inlet of the lift pump through a pipeline, and a first reaction kettle liquid discharge valve and a second reaction kettle liquid discharge valve are respectively arranged on the pipeline;
the liquid outlet of the lifting pump is connected with the liquid inlet of the complexing agent liquid preparation tank and the grease inlet of the water washing pot through pipelines, and the pipelines are respectively provided with a complexing agent liquid return valve and a grease inlet valve of the water washing pot; a liquid outlet of the complexing agent preparation tank is connected with complexing agent inlet ports of the first reaction kettle and the second reaction kettle through pipelines, and a complexing agent inlet valve of the first reaction kettle and a complexing agent inlet valve of the second reaction kettle are respectively arranged on the pipelines;
the water outlet of the hot water pot is connected with the water inlet of the water washing pot through a hot water inlet pipe, and a hot water inlet valve of the water washing pot is arranged on the hot water inlet pipe; the liquid outlet of the washing pot is connected with the liquid inlet of the fine precipitation pot through a pipeline, and a liquid outlet valve of the washing pot is arranged on the pipeline;
the fine settling pan fat outlet is connected with the low-level storage tank fat inlet through a pipeline, the fine settling pan is provided with a fine settling pan blow-off pipe, and a fine settling pan blow-off valve is arranged on the fine settling pan blow-off pipe; the liquid outlet of the low-level storage tank is connected with the liquid inlet of the distillation pump through a pipeline, and the liquid outlet of the distillation pump is connected with the grease inlet of the preheater through a pipeline; a vacuum port above the fine desilting pot is connected with a steam inlet of the condenser through a pipeline, and a vacuum valve is arranged on the pipeline;
the grease outlet of the preheater is connected with the feed inlet of the distillation still through a pipeline; the turpentine distillation outlet of the distillation pot is connected with the steam inlet of the condenser through a pipeline; a rosin outlet at the bottom of the distillation pot is connected with the fragrance releasing groove through a pipeline, and a fragrance releasing valve is arranged on the pipeline;
the steam outlet of the condenser is connected with the feed inlet of the oil-water receiver through a pipeline, and the vacuum port of the oil-water receiver is connected with the vacuum buffer tank through a pipeline; the air outlet pipe of the vacuum buffer tank is connected with the air pumping port of the vacuum pump through a vacuum pipe; the discharge port of the oil-water receiver is connected with an oil-water separator through a pipeline, the pipeline is provided with an oil-water receiver discharge valve, and the oil outlet of the oil-water separator is connected with the oil inlet of the turpentine storage tank through a pipeline; an oil outlet of the turpentine storage tank is connected with an oil inlet of a turpentine recycling pump through a pipeline, and an oil outlet of the turpentine recycling pump is connected with an oil inlet of a turpentine recycling storage tank through a pipeline.
When the device works, turpentine, tap water and turpentine in a turpentine recycling storage tank are added into a dissolving pot, stirred by steam and heated to 90 ℃, and the turpentine, the tap water and the turpentine are mixed according to the mass part ratio of 3: 1: 1; the dissolved fat liquid is pumped to a high-level pot by steam. Standing the fat liquid in an elevated kettle for 0.5 hour for coarse separation, and discharging waste water and waste residues from the bottom; discharging the lipid liquid from the discharge port to a filter for filtration. Putting the fat liquid after coarse filtration into a first reaction kettle or a second reaction kettle, adding a complexing agent solution into the reaction kettle, and stirring for 2 hours at the stirring speed of 45 revolutions per minute and the reaction temperature of 85-90 ℃; then standing for 20 minutes, after separating the lipid liquid and the complexing liquid, opening a drain valve of a first reaction kettle or a drain valve of a second reaction kettle, opening a complexing agent return valve, and pumping the complexing liquid into a complexing agent preparation tank from the bottom by using a lift pump; when the fat liquid is seen from the bottom view mirror, the complexing agent liquid return valve is closed, the fat liquid inlet valve of the washing pot is opened, the fat liquid is pumped into the washing pot, and meanwhile, hot water is opened for continuous washing operation for 10 minutes. Discharging the mixture of the washed fat liquid and the hot water into a fine precipitation pot for precipitation, and discharging the lower-layer wastewater after the fine precipitation separation from the fine precipitation pot. Putting the settled rosin into a low-level storage tank, pumping the rosin into a preheater by a distillation pump, and preheating to 140 ℃. Putting the preheated rosin into a distillation kettle for vacuum distillation; the vacuum degree is-0.07-0.08 MPa, and the distillation temperature is 165 ℃; the product remaining in the still after distillation is a food grade rosin. Vacuumizing the fine desilting pot and the distilling pot; condensing the extracted gas at a vacuum degree of-0.07 MPa to-0.08 MPa, performing oil-water separation after condensation, storing the separated oil as turpentine in a turpentine storage tank, and pumping part of the turpentine into a turpentine recycling storage tank for a dissolving process.
Example 4
The production process of the food-grade rosin comprises the following steps:
A. dissolving: adding turpentine, water and turpentine into a dissolving pot, stirring with steam, heating to dissolve to 90 ℃, and keeping the temperature for 0.5 hour, wherein the mass part ratio of the turpentine to the water to the turpentine is 3: 1: 1, conveying the dissolved rosin mixed solution to a high-level pot by steam pressure through a pipeline;
B. coarse settling and separating: carrying out coarse settling and clear separation on the dissolved rosin mixed solution in an elevated kettle, wherein settling and clear temperature is 85-90 ℃ for 0.5 hour; discharging the lower-layer wastewater after the coarse settling separation from the high-level pot; the upper layer fat liquid is put into a reaction kettle after being coarsely filtered;
C. adding a complexing agent: after the coarse precipitation and separation, feeding the supernatant lipid liquid and the complexing agent into a reaction kettle for stirring for 2 hours, wherein the stirring speed is 60 revolutions per minute, and the reaction temperature is 85-90 ℃; the mass ratio of the upper layer fat liquid to the complexing agent is 50: 3; standing for 20 minutes after the reaction is finished, and pumping the complexing agent solution into a solution preparation tank from the bottom for the next use;
D. washing with water: continuously pumping the fat liquid in the reaction kettle into a washing pot, continuously adding hot water, washing in the washing pot at a stirring speed of 60 revolutions per minute, wherein the mass part ratio of the fat liquid to the hot water is 5: 1, the temperature of hot water is 80-90 ℃; washing the fat liquor and hot water in a water washing pot for 10 minutes; discharging the mixture of the washed fat liquid and the hot water into a fine precipitation pot;
E. fine sediment separation: carrying out fine precipitation separation on the mixture of the washed fat liquid and the hot water in a fine precipitation pot for 12 hours, wherein the precipitation temperature is 85-90 ℃, and discharging the lower-layer wastewater after the fine precipitation separation from the fine precipitation pot;
F. distillation preheating: continuously pumping the settled rosin into a preheater to preheat to 140 ℃ and then discharging into a distillation boiler;
G. vacuum distillation: putting the preheated rosin into a distillation kettle for vacuum distillation for 40 minutes; the vacuum degree is-0.07-0.08 MPa, and the distillation temperature is 165 ℃; the product left in the distillation kettle after distillation is food-grade rosin;
H. and (3) turpentine recovery: vacuumizing the fine desilting pot and the distilling pot; condensing the extracted gas at vacuum degree of-0.07-0.08 MPa, separating oil from water, dissolving part of the separated oil in turpentine tank, and storing the rest in turpentine tank.
The complexing agent is an aqueous solution of ammonium fluoride, and the concentration of the aqueous solution is 0.03 mol/L.
Production equipment of food-grade rosin comprises a dissolving pot, a turpentine recycling storage tank, a batching tank, a high-level pot, a filter, a first reaction kettle, a second reaction kettle, a lift pump, a complexing agent batching tank, a washing pot, a hot water pot, a fine settling pot, a low-level storage tank, a distillation pump, a preheater, a distillation pot, a fragrance releasing tank, a condenser, an oil-water receiver, a vacuum buffer tank, a vacuum pump, an oil-water separator, a turpentine storage tank and a turpentine oil recovery pump;
the turpentine inlet oil port of the dissolving pot is connected with the oil outlet of the turpentine recycling storage tank through a pipeline, and a turpentine liquid inlet valve is arranged on the pipeline; the feed port of the dissolving pot is connected with the batching tank through a pipeline, and a feed valve is arranged on the pipeline; the water inlet of the dissolving pot is connected through a tap water pipe, and a water inlet valve of the dissolving pot is arranged on the tap water pipe; the liquid outlet of the dissolving pot is connected with the feed inlet of the high-level pot through a material pipeline, and a material valve is arranged on the material pipe; a steam pipeline is arranged on the dissolving pot, and a steam inlet valve is arranged on the steam pipeline;
the high-level pot discharging port is connected with the liquid inlet of the filter through a pipeline, and a high-level pot discharging valve is arranged on the pipeline; the lower part of the high-level pot is provided with a high-level pot blow-off pipe which is provided with a high-level pot blow-off valve;
the liquid outlet of the filter is respectively connected with the grease inlets of the first reaction kettle and the second reaction kettle through pipelines, and the pipelines are provided with a grease inlet valve of the first reaction kettle and a grease inlet valve of the second reaction kettle; the bottom of the reaction kettle is connected with a liquid inlet of the lift pump through a pipeline, and a first reaction kettle liquid discharge valve and a second reaction kettle liquid discharge valve are respectively arranged on the pipeline;
the liquid outlet of the lifting pump is connected with the liquid inlet of the complexing agent liquid preparation tank and the grease inlet of the water washing pot through pipelines, and the pipelines are respectively provided with a complexing agent liquid return valve and a grease inlet valve of the water washing pot; a liquid outlet of the complexing agent preparation tank is connected with complexing agent inlet ports of the first reaction kettle and the second reaction kettle through pipelines, and a complexing agent inlet valve of the first reaction kettle and a complexing agent inlet valve of the second reaction kettle are respectively arranged on the pipelines;
the water outlet of the hot water pot is connected with the water inlet of the water washing pot through a hot water inlet pipe, and a hot water inlet valve of the water washing pot is arranged on the hot water inlet pipe; the liquid outlet of the washing pot is connected with the liquid inlet of the fine precipitation pot through a pipeline, and a liquid outlet valve of the washing pot is arranged on the pipeline;
the fine settling pan fat outlet is connected with the low-level storage tank fat inlet through a pipeline, the fine settling pan is provided with a fine settling pan blow-off pipe, and a fine settling pan blow-off valve is arranged on the fine settling pan blow-off pipe; the liquid outlet of the low-level storage tank is connected with the liquid inlet of the distillation pump through a pipeline, and the liquid outlet of the distillation pump is connected with the grease inlet of the preheater through a pipeline; a vacuum port above the fine desilting pot is connected with a steam inlet of the condenser through a pipeline, and a vacuum valve is arranged on the pipeline;
the grease outlet of the preheater is connected with the feed inlet of the distillation still through a pipeline; the turpentine distillation outlet of the distillation pot is connected with the steam inlet of the condenser through a pipeline; a rosin outlet at the bottom of the distillation pot is connected with the fragrance releasing groove through a pipeline, and a fragrance releasing valve is arranged on the pipeline;
the steam outlet of the condenser is connected with the feed inlet of the oil-water receiver through a pipeline, and the vacuum port of the oil-water receiver is connected with the vacuum buffer tank through a pipeline; the air outlet pipe of the vacuum buffer tank is connected with the air pumping port of the vacuum pump through a vacuum pipe; the discharge port of the oil-water receiver is connected with an oil-water separator through a pipeline, the pipeline is provided with an oil-water receiver discharge valve, and the oil outlet of the oil-water separator is connected with the oil inlet of the turpentine storage tank through a pipeline; an oil outlet of the turpentine storage tank is connected with an oil inlet of a turpentine recycling pump through a pipeline, and an oil outlet of the turpentine recycling pump is connected with an oil inlet of a turpentine recycling storage tank through a pipeline.
When the device works, turpentine, tap water and turpentine in a turpentine recycling storage tank are added into a dissolving pot, stirred by steam and heated to 90 ℃, and the turpentine, the tap water and the turpentine are mixed according to the mass part ratio of 3: 1: 1; the dissolved fat liquid is pumped to a high-level pot by steam. Standing the fat liquid in an elevated kettle for 0.5 hour for coarse separation, and discharging waste water and waste residues from the bottom; discharging the lipid liquid from the discharge port to a filter for filtration. Putting the fat liquid after coarse filtration into a first reaction kettle or a second reaction kettle, adding a complexing agent solution into the reaction kettle, and stirring for 2 hours at the stirring speed of 60 revolutions per minute and the reaction temperature of 85-90 ℃; then standing for 20 minutes, after separating the lipid liquid and the complexing liquid, opening a drain valve of a first reaction kettle or a drain valve of a second reaction kettle, opening a complexing agent return valve, and pumping the complexing liquid into a complexing agent preparation tank from the bottom by using a lift pump; when the fat liquid is seen from the bottom view mirror, the complexing agent liquid return valve is closed, the fat liquid inlet valve of the washing pot is opened, the fat liquid is pumped into the washing pot, and meanwhile, hot water is opened for continuous washing operation for 10 minutes. Discharging the mixture of the washed fat liquid and the hot water into a fine precipitation pot for precipitation, and discharging the lower-layer wastewater after the fine precipitation separation from the fine precipitation pot. Putting the settled rosin into a low-level storage tank, pumping the rosin into a preheater by a distillation pump, and preheating to 140 ℃. Putting the preheated rosin into a distillation kettle for vacuum distillation; the vacuum degree is-0.07-0.08 MPa, and the distillation temperature is 165 ℃; the product remaining in the still after distillation is a food grade rosin. Vacuumizing the fine desilting pot and the distilling pot; condensing the extracted gas at a vacuum degree of-0.07 MPa to-0.08 MPa, performing oil-water separation after condensation, storing the separated oil as turpentine in a turpentine storage tank, and pumping part of the turpentine into a turpentine recycling storage tank for a dissolving process.
Claims (1)
1. Production equipment of food-grade rosin is characterized by comprising a dissolving pot (1), a turpentine recycling storage tank (2), a dosing tank (3), a high-level pot (4), a filter (5), a first reaction kettle (6), a second reaction kettle (7), a lifting pump (8), a complexing agent dosing tank (9), a washing pot (10), a hot water pot (11), a fine settling pot (12), a low-level storage tank (13), a distillation pump (14), a preheater (15), a distillation pot (16), a fragrance releasing tank (17), a condenser (18), an oil-water receiver (19), a vacuum buffer tank (20), a vacuum pump (21), an oil-water separator (22), a turpentine storage tank (23) and a turpentine recycling pump (24);
the turpentine inlet oil port of the dissolving pot (1) is connected with the oil outlet of the turpentine recycling storage tank (2) through a pipeline, and a turpentine inlet valve (25) is arranged on the pipeline; the feed inlet of the dissolving pot (1) is connected with the batching tank (3) through a pipeline, and a feed valve (26) is arranged on the pipeline; the water inlet of the dissolving pot (1) is connected through a tap water pipe, and a water inlet valve (27) of the dissolving pot is arranged on the tap water pipe; the liquid outlet of the dissolving pot (1) is connected with the feed inlet of the high-level pot (4) through a material pipeline, and a material valve (28) is arranged on the material pipeline; a steam pipeline (29) is arranged on the dissolving pot (1), and a steam inlet valve (30) is arranged on the steam pipeline (29);
the discharge port of the high-level pot (4) is connected with the liquid inlet of the filter (5) through a pipeline, and a discharge valve (31) of the high-level pot is arranged on the pipeline; a high-level pot blow-off pipe (32) is arranged at the lower part of the high-level pot (4), and a high-level pot blow-off valve (33) is arranged on the high-level pot blow-off pipe (32);
a liquid outlet of the filter (5) is respectively connected with a grease inlet of the first reaction kettle (6) and a grease inlet of the second reaction kettle (7) through pipelines, and a grease inlet valve (34) of the first reaction kettle and a grease inlet valve (35) of the second reaction kettle are arranged on the pipelines; the bottom of the reaction kettle is connected with a liquid inlet of a lift pump (8) through a pipeline, and a first reaction kettle liquid discharge valve (36) and a second reaction kettle liquid discharge valve (37) are respectively arranged on the pipeline;
a liquid outlet of the lift pump (8) is connected with a liquid inlet of the complexing agent liquid preparation tank (9) and a grease inlet of the water washing pot (10) through pipelines, and a complexing agent liquid return valve (38) and a grease inlet valve (39) of the water washing pot are respectively arranged on the pipelines; a liquid outlet of the complexing agent preparation tank (9) is connected with complexing agent inlet ports of the first reaction kettle (6) and the second reaction kettle (7) through pipelines, and a complexing agent inlet valve (40) of the first reaction kettle and a complexing agent inlet valve (41) of the second reaction kettle are respectively arranged on the pipelines;
the water outlet of the hot water pot (11) is connected with the water inlet of the water washing pot (10) through a hot water inlet pipe, and a hot water inlet valve (42) of the water washing pot is arranged on the hot water inlet pipe; a liquid outlet of the washing pot (10) is connected with a liquid inlet of the fine sedimentation pot (12) through a pipeline, and a liquid outlet valve (43) of the washing pot is arranged on the pipeline;
a fat liquid outlet of the fine desilting pot (12) is connected with a fat inlet of the low-level storage tank (13) through a pipeline, the fine desilting pot (12) is provided with a fine desilting pot drain pipe (44), and a fine desilting pot drain valve (45) is arranged on the fine desilting pot drain pipe (44); a liquid outlet of the low-level storage tank (13) is connected with a liquid inlet of a distillation pump (14) through a pipeline, and a liquid outlet of the distillation pump (14) is connected with a grease inlet of a preheater (15) through a pipeline; a vacuum port above the fine precipitation pot (12) is connected with a steam inlet of the condenser (18) through a pipeline, and a vacuum valve (46) is arranged on the pipeline;
the grease outlet of the preheater (15) is connected with the feed inlet of the distillation pot (16) through a pipeline; the turpentine distillation outlet of the distillation pot (16) is connected with the steam inlet of the condenser (18) through a pipeline; a rosin outlet at the bottom of the distillation pot (16) is connected with the fragrance releasing groove (17) through a pipeline, and a fragrance releasing valve (47) is arranged on the pipeline;
a steam outlet of the condenser (18) is connected with a feed inlet of the oil-water receiver (19) through a pipeline, and a vacuum port of the oil-water receiver (19) is connected with a vacuum buffer tank (20) through a pipeline; the air outlet pipe of the vacuum buffer tank (20) is connected with the air extraction opening of the vacuum pump (21) through a vacuum pipe; the discharge hole of the oil-water receiver (19) is connected with the oil-water separator (22) through a pipeline, an oil-water receiver discharge valve (48) is arranged on the pipeline, and the oil outlet of the oil-water separator (22) is connected with the oil inlet of the turpentine storage tank (23) through a pipeline; an oil outlet of the turpentine storage tank (23) is connected with an oil inlet of a turpentine recycling pump (24) through a pipeline, and an oil outlet of the turpentine recycling pump (24) is connected with an oil inlet of the turpentine recycling storage tank (2) through a pipeline.
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| CN112457779A (en) * | 2020-11-19 | 2021-03-09 | 广西壮族自治区林业科学研究院 | Water-white heat stability rosin resin production equipment |
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Denomination of invention: Production process and equipment of food grade rosin Effective date of registration: 20230620 Granted publication date: 20201124 Pledgee: Yuxi Branch of Postal Savings Bank of China Co.,Ltd. Pledgor: YUNNAN LINYUAN SPICES CO.,LTD. Registration number: Y2023980045104 |