CN105418414A - Production method for glycerol monostearate and glycerol distearate - Google Patents
Production method for glycerol monostearate and glycerol distearate Download PDFInfo
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- CN105418414A CN105418414A CN201510976034.9A CN201510976034A CN105418414A CN 105418414 A CN105418414 A CN 105418414A CN 201510976034 A CN201510976034 A CN 201510976034A CN 105418414 A CN105418414 A CN 105418414A
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- stearin
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/03—Preparation of carboxylic acid esters by reacting an ester group with a hydroxy group
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- 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
- C11B3/10—Refining fats or fatty oils by adsorption
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
- C11C3/06—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils with glycerol
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
- C11C3/10—Ester interchange
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
The invention provides a production method for glycerol monostearate and glycerol distearate. The production method comprises the following steps: with hydrogenated oil and glycerol as raw materials, sodium stearate as a catalyst and nitrogen gas as protective gas, carrying out transesterification reaction in a transesterification reactor with vacuum pressure to be minus 0.097 Mpa and reaction temperature to be controlled at 220 to 260 DEG C, and after the reaction is completed, subjecting reaction materials to quenching so as to obtain glycerol monostearate and glycerol distearate. According to the invention, through the adsorption effect of an arranged decolorizing kettle to pigments of the hydrogenated oil, a part of the pigments can be removed, so the oil achieves the requirements of production; meanwhile, the process of premixing is adopted, and two esterification reactors are utilized, so heat transfer process can be carried out, and heat energy is completely recycled and utilized; the proportions of sodium stearate, glycerol and hydrogenated oil are limited, and all control points are controlled; thus, glycerol monostearate and glycerol distearate which are suitable for being added into food are obtained.
Description
Technical field
The invention belongs to foodstuff additive field, particularly relate to the production method of the single, double stearin of additive.
Background technology
Single, double Vinlub is nonionic emulsifier, HLB value 2.5-3.0.Be approved as food emulsifier in " foodstuff additive use hygienic standard " (GB2760-2007), can use in right amount by need of production in varieties of food items; And can at original flavor fermented-milk (full-cream, partially skimmed, degreasing), rare cream, butter and concentrated butter, raw wet, raw dried noodle goods, syrup, spice, uses in the products such as coffee drinks class.
Along with the fast development of China's daily use chemicals, food service industry, the demand of single, double stearin is increasing, in order to meet the demand that mono-glycerides consumption increases day by day, prepare with lower cost the emphasis that highly purified single, double stearin becomes this area research.
Summary of the invention
The object of this invention is to provide the production method of a kind of high yield, high quality, low cost, easy industrialized single, double stearin.
For realizing goal of the invention, the technical scheme that the present invention takes is:
A kind of production method of single, double stearin; comprise with winterized stearin and glycerine for raw material carries out transesterification reaction in transesterification reactor; employing sodium stearate is catalyzer; the vacuum pressure of reaction is-0.097Mpa; temperature of reaction controls at 220 ~ 260 DEG C; nitrogen is shielding gas; after reaction terminates; chilling is carried out to reaction mass and obtains single, double stearin; the weight of described glycerine is the 20%-25% of winterized stearin weight, and the weight of sodium stearate is the 0.05%-0.1% of winterized stearin and glycerine gross weight.
As preferably, also comprise in this production method and winterized stearin is processed: with vacuum pump, winterized stearin is sucked into Decolouring pot, open and stir, steam is warming up to 90 DEG C ~ 100 DEG C, vacuum hydro-extraction about 15 ~ 20 minutes, sucks in Decolouring pot by the discoloring agent prepared, stirring is warming up to 100 DEG C ~ 120 DEG C, utilize pressurized air to be filtered by plate-and-frame filter press by the material in Decolouring pot, the winterized stearin after decolorization filtering is put into medial launder, be delivered to winterized stearin metering pool.
Concrete, the production method of a kind of single, double stearin of the present invention, comprises the steps:
1) winterized stearin is processed: with vacuum pump, winterized stearin is sucked into Decolouring pot, open and stir, steam is warming up to 90 DEG C ~ 100 DEG C, vacuum hydro-extraction about 15 ~ 20 minutes, the discoloring agent prepared is sucked in Decolouring pot, stirs and be warming up to 100 DEG C ~ 120 DEG C, utilize pressurized air to be filtered by plate-and-frame filter press by the material in Decolouring pot, winterized stearin after decolorization filtering is put into medial launder, is delivered to winterized stearin metering pool;
2) pre-mixing: with toothed gear pump by the glycerine in the winterized stearin in winterized stearin metering pool and glycerine pond, get in mixing kettle respectively by mass flowmeter, open and stir pre-mixing, treat that liquid level arrives unloading position, open mixing kettle discharging pump, be driven into by the material mixed in esterifying kettle 1#, discharging pump is by liquid automatic control pump control speed;
3) transesterification reaction: under vacuum conditions, sodium stearate toothed gear pump is got in esterifying kettle 1# by under meter, heat-conducting oil heating is utilized to heat up, should not stop during heating to stir, be warming up to 220 ~ 250 DEG C, inflated with nitrogen during reaction, still 1# liquid level to be esterified reaches unloading position, open mixing kettle 1# discharging pump, discharging pump is by the speed of liquid automatic control pump, the material of esterifying kettle 1# is driven in esterifying kettle 2#, continue heated and stirred temperature reaction, be warming up to 240 ~ 260 DEG C, inflated with nitrogen during reaction, when reaction becomes clear solution to solution, transesterification reaction completes.
4) still 2# liquid level to be esterified reaches unloading position, and open esterifying kettle 2# discharging pump, completely reacted material, by the speed of liquid automatic control pump, is carried out chilling by water cooler, enters finished product header tank after being cooled to 100 ~ 120 DEG C by discharging pump;
5) in finished product header tank, continue material to be cooled to 100 DEG C below, then carry out watering dish or chill roles scraping blade shaping, test package.
As preferably, described step 1) in discoloring agent be atlapulgite.
As preferably, described step 2) in be filled with nitrogen, nitrogen pressure must not more than 0.1Mpa.
As preferably, the weight of glycerine is the 20%-25% of winterized stearin weight, and the weight of sodium stearate is the 0.05%-0.1% of winterized stearin and glycerine gross weight.
The present invention is about a kind of production method of single, double stearin, by being provided with decolouring still to the adsorption of the pigment of winterized stearin, wherein partial pigment can be removed, grease is made to reach production requirement, adopt the technology utilization 2 of pre-mixing to overlap esterifying kettle simultaneously, can heat transfer process be carried out, fully heat energy be recycled, the control of restriction and each reference mark is carried out to the ratio of sodium stearate, glycerine and winterized stearin, has obtained a kind of single, double stearin meeting food and add.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
1) winterized stearin is processed: with vacuum pump, winterized stearin is sucked into Decolouring pot, open and stir, steam is warming up to 90 DEG C, vacuum hydro-extraction about 15 minutes, the atlapulgite prepared is sucked in Decolouring pot, stirs and be warming up to 100 DEG C, utilize pressurized air to be filtered by plate-and-frame filter press by the material in Decolouring pot, winterized stearin after decolorization filtering is put into medial launder, is delivered to winterized stearin metering pool;
2) pre-mixing: with toothed gear pump by the winterized stearin 200kg in winterized stearin metering pool and the glycerine 40kg in glycerine pond, get in mixing kettle respectively by mass flowmeter, open and stir pre-mixing, treat that liquid level arrives unloading position, open mixing kettle discharging pump, be driven into by the material mixed in esterifying kettle 1#, discharging pump is by liquid automatic control pump control speed;
3) transesterification reaction: under vacuum conditions, sodium stearate 12kg toothed gear pump is got in esterifying kettle 1# by under meter, heat-conducting oil heating is utilized to heat up, should not stop during heating to stir, be warming up to 220 DEG C, inflated with nitrogen during reaction, still 1# liquid level to be esterified reaches unloading position, open mixing kettle 1# discharging pump, discharging pump is by the speed of liquid automatic control pump, the material of esterifying kettle 1# is driven in esterifying kettle 2#, continue heated and stirred temperature reaction, be warming up to 240 DEG C, inflated with nitrogen during reaction, nitrogen pressure is 0.08Mpa, when reaction becomes clear solution to solution, transesterification reaction completes.
4) still 2# liquid level to be esterified reaches unloading position, and open esterifying kettle 2# discharging pump, completely reacted material, by the speed of liquid automatic control pump, is carried out chilling by water cooler, enters finished product header tank after being cooled to 100 DEG C by discharging pump;
5) in finished product header tank, continue material to be cooled to 100 DEG C below, then carry out watering dish or chill roles scraping blade shaping, finally pack.
Embodiment 2
1) winterized stearin is processed: with vacuum pump, winterized stearin is sucked into Decolouring pot, open and stir, steam is warming up to 100 DEG C, vacuum hydro-extraction about 15 minutes, the atlapulgite prepared is sucked in Decolouring pot, stirs and be warming up to 100 DEG C, utilize pressurized air to be filtered by plate-and-frame filter press by the material in Decolouring pot, winterized stearin after decolorization filtering is put into medial launder, is delivered to winterized stearin metering pool;
2) pre-mixing: with toothed gear pump by the winterized stearin 200kg in winterized stearin metering pool and the glycerine 50kg in glycerine pond, get in mixing kettle respectively by mass flowmeter, open and stir pre-mixing, treat that liquid level arrives unloading position, open mixing kettle discharging pump, be driven into by the material mixed in esterifying kettle 1#, discharging pump is by liquid automatic control pump control speed;
3) transesterification reaction: under vacuum conditions, sodium stearate 25kg toothed gear pump is got in esterifying kettle 1# by under meter, heat-conducting oil heating is utilized to heat up, should not stop during heating to stir, be warming up to 240 DEG C, inflated with nitrogen during reaction, still 1# liquid level to be esterified reaches unloading position, open mixing kettle 1# discharging pump, discharging pump is by the speed of liquid automatic control pump, the material of esterifying kettle 1# is driven in esterifying kettle 2#, continue heated and stirred temperature reaction, be warming up to 260 DEG C, inflated with nitrogen during reaction, nitrogen pressure is 0.1Mpa, when reaction becomes clear solution to solution, transesterification reaction completes.
4) still 2# liquid level to be esterified reaches unloading position, and open esterifying kettle 2# discharging pump, completely reacted material, by the speed of liquid automatic control pump, is carried out chilling by water cooler, enters finished product header tank after being cooled to 110 DEG C by discharging pump;
5) in finished product header tank, continue material to be cooled to 100 DEG C below, then carry out watering dish or chill roles scraping blade shaping, test package.
Embodiment 3
1) winterized stearin is processed: with vacuum pump, winterized stearin is sucked into Decolouring pot, open and stir, steam is warming up to 95 DEG C, vacuum hydro-extraction about 20 minutes, the atlapulgite prepared is sucked in Decolouring pot, stirs and be warming up to 120 DEG C, utilize pressurized air to be filtered by plate-and-frame filter press by the material in Decolouring pot, winterized stearin after decolorization filtering is put into medial launder, is delivered to winterized stearin metering pool;
2) pre-mixing: with toothed gear pump by the winterized stearin 200kg in winterized stearin metering pool and the glycerine 44kg in glycerine pond, get in mixing kettle respectively by mass flowmeter, open and stir pre-mixing, treat that liquid level arrives unloading position, open mixing kettle discharging pump, be driven into by the material mixed in esterifying kettle 1#, discharging pump is by liquid automatic control pump control speed;
3) transesterification reaction: under vacuum conditions, sodium stearate 19.52kg toothed gear pump is got in esterifying kettle 1# by under meter, heat-conducting oil heating is utilized to heat up, should not stop during heating to stir, be warming up to 230 DEG C, inflated with nitrogen during reaction, still 1# liquid level to be esterified reaches unloading position, open mixing kettle 1# discharging pump, discharging pump is by the speed of liquid automatic control pump, the material of esterifying kettle 1# is driven in esterifying kettle 2#, continue heated and stirred temperature reaction, be warming up to 250 DEG C, inflated with nitrogen during reaction, nitrogen pressure is 0.05Mpa, when reaction becomes clear solution to solution, transesterification reaction completes.
4) still 2# liquid level to be esterified reaches unloading position, and open esterifying kettle 2# discharging pump, completely reacted material, by the speed of liquid automatic control pump, is carried out chilling by water cooler, enters finished product header tank after being cooled to 120 DEG C by discharging pump;
5) in finished product header tank, continue material to be cooled to 100 DEG C below, then carry out watering dish or chill roles scraping blade shaping, test package.
Index analysis is carried out to the product of above-described embodiment, the results are shown in Table:
Claims (5)
1. the production method of a single, double stearin; it is characterized in that comprising with winterized stearin and glycerine for raw material carries out transesterification reaction in transesterification reactor; employing sodium stearate is catalyzer; the vacuum pressure of reaction is-0.097Mpa; temperature of reaction controls at 220 ~ 260 DEG C; nitrogen is shielding gas; after reaction terminates; chilling is carried out to reaction mass and obtains single, double stearin; the weight of described glycerine is the 20%-25% of winterized stearin weight, and the weight of sodium stearate is 0.05% ~ 0.1% of winterized stearin and glycerine gross weight.
2. the production method of a kind of single, double stearin according to claim 1, characterized by further comprising and winterized stearin is processed: with vacuum pump, winterized stearin is sucked into Decolouring pot, open and stir, steam is warming up to 90 DEG C ~ 100 DEG C, vacuum hydro-extraction about 15 ~ 20 minutes, the discoloring agent prepared is sucked in Decolouring pot, stirring is warming up to 100 DEG C ~ 120 DEG C, pressurized air is utilized to be filtered by plate-and-frame filter press by the material in Decolouring pot, winterized stearin after decolorization filtering is put into medial launder, is delivered to winterized stearin metering pool.
3. the production method of a kind of single, double stearin according to claim 1 is concrete, it is characterized in that comprising the steps:
1) winterized stearin is processed: with vacuum pump, winterized stearin is sucked into Decolouring pot, open and stir, steam is warming up to 90 DEG C ~ 100 DEG C, vacuum hydro-extraction about 15 ~ 20 minutes, the discoloring agent prepared is sucked in Decolouring pot, stirs and be warming up to 100 DEG C ~ 120 DEG C, utilize pressurized air to be filtered by plate-and-frame filter press by the material in Decolouring pot, winterized stearin after decolorization filtering is put into medial launder, is delivered to winterized stearin metering pool;
2) pre-mixing: with toothed gear pump by the glycerine in the winterized stearin in winterized stearin metering pool and glycerine pond, get in mixing kettle respectively by mass flowmeter, open and stir pre-mixing, treat that liquid level arrives unloading position, open mixing kettle discharging pump, be driven into by the material mixed in esterifying kettle 1#, discharging pump is by liquid automatic control pump speed;
3) transesterification reaction: under vacuum conditions, sodium stearate toothed gear pump is got in esterifying kettle 1# by under meter, heat-conducting oil heating is utilized to heat up, should not stop during heating to stir, be warming up to 220 ~ 250 DEG C, inflated with nitrogen during reaction, still 1# liquid level to be esterified reaches unloading position, open mixing kettle 1# discharging pump, discharging pump is by the speed of liquid automatic control pump, the material of esterifying kettle 1# is driven in esterifying kettle 2#, continue heated and stirred temperature reaction, be warming up to 240 ~ 260 DEG C, inflated with nitrogen during reaction, when reaction becomes clear solution to solution, transesterification reaction completes.
4) still 2# liquid level to be esterified reaches unloading position, and open esterifying kettle 2# discharging pump, completely reacted material, by the speed of liquid automatic control pump, is carried out chilling by water cooler, enters finished product header tank after being cooled to 100 ~ 120 DEG C by discharging pump;
5) in finished product header tank, continue material to be cooled to 100 DEG C below, then carry out watering dish or chill roles scraping blade shaping, test package.
4. the production method of a kind of single, double stearin according to Claims 2 or 3, is characterized in that described discoloring agent is atlapulgite.
5. the production method of a kind of single, double stearin according to claim 3, is characterized in that the nitrogen pressure in described step 3 must not more than 0.1Mpa.
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CN201510976034.9A CN105418414B (en) | 2015-12-22 | 2015-12-22 | A kind of production method of single, double tristerin |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106565483A (en) * | 2016-11-04 | 2017-04-19 | 杭州油脂化工有限公司 | Two-step method of producing glyceryl monostearate and glyceryl distearate with low free glycerol |
CN112679344A (en) * | 2020-12-29 | 2021-04-20 | 浙江物美生物科技有限公司 | Preparation process of monoglyceride |
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US6127561A (en) * | 1997-08-19 | 2000-10-03 | Global Palm Products Sdn. Bhd. | Process for the production of monoglyceride based on the glycerolysis of methyl ester |
CN101967095A (en) * | 2010-08-20 | 2011-02-09 | 骆增来 | 12-hydroxyl stearic acid glyceride as well as preparation method and application thereof |
CN102876464A (en) * | 2012-09-05 | 2013-01-16 | 南昌大学 | Process for preparing high-purity molecular distillation monoacylglycerol |
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2015
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Patent Citations (4)
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CN1076187A (en) * | 1993-01-19 | 1993-09-15 | 周端午 | The preparation method of high-purity monostearin |
US6127561A (en) * | 1997-08-19 | 2000-10-03 | Global Palm Products Sdn. Bhd. | Process for the production of monoglyceride based on the glycerolysis of methyl ester |
CN101967095A (en) * | 2010-08-20 | 2011-02-09 | 骆增来 | 12-hydroxyl stearic acid glyceride as well as preparation method and application thereof |
CN102876464A (en) * | 2012-09-05 | 2013-01-16 | 南昌大学 | Process for preparing high-purity molecular distillation monoacylglycerol |
Non-Patent Citations (1)
Title |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106565483A (en) * | 2016-11-04 | 2017-04-19 | 杭州油脂化工有限公司 | Two-step method of producing glyceryl monostearate and glyceryl distearate with low free glycerol |
CN106565483B (en) * | 2016-11-04 | 2018-12-14 | 杭州油脂化工有限公司 | A kind of method that two-step method prepares the low single, double tristerin of dissociative glycerin |
CN112679344A (en) * | 2020-12-29 | 2021-04-20 | 浙江物美生物科技有限公司 | Preparation process of monoglyceride |
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Denomination of invention: A production method of monostearin and bistearin Effective date of registration: 20210824 Granted publication date: 20170825 Pledgee: Zhejiang Fuyang rural commercial bank Limited by Share Ltd. Dongzhou branch Pledgor: HANGZHOU FUCHUN FOOD ADDITIVE Co.,Ltd. Registration number: Y2021330001221 |
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