CN102352222A - Preparation method of biomass based antifreeze fluid mother liquor - Google Patents
Preparation method of biomass based antifreeze fluid mother liquor Download PDFInfo
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- CN102352222A CN102352222A CN2011102302623A CN201110230262A CN102352222A CN 102352222 A CN102352222 A CN 102352222A CN 2011102302623 A CN2011102302623 A CN 2011102302623A CN 201110230262 A CN201110230262 A CN 201110230262A CN 102352222 A CN102352222 A CN 102352222A
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Abstract
The invention provides a preparation method of a biomass based antifreeze fluid mother liquor. The antifreeze fluid mother liquor is a reddish transparent liquid, and blending of the antifreeze fluid needs no artificial warning pigment. The antifreeze fluid mother liquor has poly sugar alcohol as the main component and has no pollution to the environment. The antifreeze fluid mother liquor has a freezing point of -70-75DEG C and a boiling point of 110DEG C-118DEG C. The prepared antifreeze fluid has better antifreeze effect than glycol. A 50% aqueous solution prepared by glycol has a freezing point of -37DEG C, while a 50% aqueous solution prepared by the biomass based antifreeze fluid mother liquor prepared in the invention has a freezing point of -50DEG C. The method for preparing a biomass based antifreeze fluid mother liquor in the invention has low production cost, wide raw material sources, and simple production process, thus being able to be widely used in antifreeze fluid mother liquor production.
Description
Technical field
The invention provides a kind of preparation method of biomass-based deicing fluid mother liquor, relate to the method for the synthetic polyvalent alcohol of monose catalyzed degradation, belong to the biomass technical field.
Background technology
Deicing fluid has stronger frost resistance, can be noncondensing in the environment of subzero tens degree, keep good flowability; Have higher boiling point simultaneously, can lower the temperature to carrier, it is overheated to prevent.Thereby has a good temperature adjusting performance.On being applied in motor car engine, also be applied in numerous areas such as train, ships, aircraft, sun power, Nuclear power plants, industrial processes, military and national defense, communications and transportation, Coal Transport, aircraft, airstrip and road deicing widely, year consumption is very big.
At present, it is main raw material that terepthaloyl moietie is generally adopted in countries in the world deicing fluid production, adds allotments such as pure water, tinting material, inhibiter, defoamer, mould inhibitor, buffer reagent and forms.
There are many shortcoming and defect in this deicing fluid mode of production: 1, terepthaloyl moietie is the derived prods of petroleum products, and its raw materials for production are non-renewable.2, terepthaloyl moietie is of many uses is chemical industry synthetic main raw material, and being used on the deicing fluid product is a kind of loss and waste and caving-in bash of resource; 3, terepthaloyl moietie is poisonous, and the people wrongly takes for preventing as deicing fluid if clothes are gone into the millesimal amount of body weight can cause death, and needs to add artificial color with caution.4, terepthaloyl moietie is to be difficult for decomposing contaminate environment behind the discharging of waste liquid of deicing fluid of raw material; 5, terepthaloyl moietie scarcity of resources price is high, and it is violent to change fluctuation with international oil price, directly influences the production of deicing fluid and stablizing of market.(reference: " 2010-2014 ethylene glycol type deicing fluid industry market competition situation and invest money in developing strategy report ", chin or cheek Hua Sheng Science and Technology Ltd. of Beijing army; " Chinese deicing fluid market intelligence ", Beijing thousand news chemical combination information are addressed inquires to company limited).
At present, have the deicing fluid of particular criteria the glycerin used also to be arranged as raw material production to some, but its price is expensive more, is the several times of ethylene glycol antifreeze price, nots get along well economically, can not generally use.(" 2009 domestic and international glycerin deicing fluid market analysis and prediction address ", company limited is addressed inquires in Beijing Li Desipu business administration).
The substitute products that find a kind of terepthaloyl moietie raw material are needed in above situation explanation badly, and its standard is: the sustainable use of aboundresources; Cheap good economy performance, the simple and direct easy realization of technology, product quality and performances are better.
Summary of the invention
The object of the invention is to provide a kind of preparation method of biomass-based deicing fluid mother liquor, substitutes petroleum products terepthaloyl moietie with renewable raw materials and produces biomass-based deicing fluid, and the deicing fluid starting material are in short supply to solve, toxicity and deicing fluid problem on the high side.
The preparation method of a kind of biomass-based deicing fluid mother liquor provided by the invention, its prescription is: (1) raw materials of glucose or starch quality are 100 parts; (2) the catalyzer nickel salt is a kind of of nickel acetate, Hydrocerol A nickel, nickel formate or acetylacetonate nickel; The amount of catalyzer is the 0.44-0.80% of raw materials quality; (3) phase-transfer catalyst is PPG-200, PPG-400 or PPG-600; Its consumption is that 1.11-2.00% (4) oxidation inhibitor of raw materials quality is p-NP, thiodiphenylamine or 4010-NA, and consumption is that 0.44-0.80% (5) the auxiliary agent sodium formiate consumption of raw materials quality is the 27.49-30.4% of raw materials quality;
By proportioning; The adding mass concentration is 45.0% glucose or amidin in the reaction kettle that has heating temperature control, whipping appts, and mass concentration is 35.0% sodium formate solution, catalyst acetic acid nickel; Phase-transfer catalyst; Add thermo-stabilizer again, antioxidant stirs; Reacted 2-4 hour down at 90-110 ℃; Cool to 30 ℃, after ion-exchange, make a kind of biomass-based deicing fluid mother liquor.It is the transparent liquid of blush, freezing point is-and 70-75 ℃.
Beneficial effect: a kind of biomass-based deicing fluid mother liquor that (1) the present invention makes, be blush transparent liquid arranged, allotment deicing fluid need not add artificial caution pigment; (2) deicing fluid mother liquor main component is multi-sugar alcohol, and is free from environmental pollution; (3) a kind of biomass-based deicing fluid mother liquor freezing point that makes of the present invention is-70-75 ℃, and boiling point is the 110-118 degree.A kind of biomass-based deicing fluid mother liquor with the present invention makes is prepared deicing fluid; Antifreezing effect is better than terepthaloyl moietie; It is-37 ℃ that terepthaloyl moietie is modulated 50% aqueous solution freezing point, and the freezing point that a kind of biomass-based deicing fluid mother liquor that makes with the present invention is modulated 50% aqueous solution is-50 ℃; (4) production cost is low, processes biomass-based deicing fluid mother liquor production cost by the inventive method: about 1800 yuan per ton, and can modulate 2.0 tons of freezing points and be-50 ℃ deicing fluid, the market price is more than 20,000 yuan.And 1.2 ten thousand yuan of the expenses of the required terepthaloyl moietie of deicing fluid of production equivalent.Through detecting, the performance of the deicing fluid prepared of mother liquor and technical indicator satisfy more than the condensation point-45 that CNS stipulates ℃ fully thus, and boiling point is more than 108 ℃.The present invention has the advantages that raw material sources are wide, production process is simple, product performance are good and market application foreground is wide.The alternative terepthaloyl moietie of product is as the mother liquor of producing deicing fluid.
Embodiment
Embodiment 1 has that to add 38.0 gram mass concentration in the 250ml reaction kettle of heating temperature control, whipping appts be 45.0% D/W, and glucose quality is 17.1 grams; Mass concentration is 35.0% sodium formate solution 13.3 grams, and the sodium formiate quality is 4.7 grams; Catalyst acetic acid nickel 0.076 gram, phase-transfer catalyst PPG-2000.19 gram; Add thermo-stabilizer Resorcinol 0.076 gram, antioxidant p-NP 0.076 gram again; Stir; Make above-mentioned raw materials 90 ℃ of reactions 2 hours; Lower the temperature after 30 ℃; Through ion exchange treatment, process biomass-based deicing fluid mother liquor, freezing point is-72 ℃.
Embodiment 2 adding 38.0 gram mass concentration in the 250ml reaction kettle that has heating temperature control, whipping appts are 47.0% amidin, and mass concentration is 37.0% sodium formate solution 13.68 grams, and the sodium formiate quality is 5.062 grams; Catalyzer Hydrocerol A nickel 0.114 gram, phase-transfer catalyst PPG-400 0.266 gram; Add thermo-stabilizer Resorcinol 0.114 gram, antioxidant thiodiphenylamine 0.114 gram again; Stir; Make above-mentioned raw materials 105 ℃ of reactions 3 hours; Lower the temperature after 30 ℃; Through ion exchange treatment, process biomass-based deicing fluid mother liquor.Freezing point-75 ℃.
Embodiment 3 adding 38 gram mass concentration in the 250ml reaction kettle that has heating temperature control, whipping appts are 50.0% amidin, and starch quality is 17.86 grams, and mass concentration is 40.0% sodium formate solution 14.44 grams, and the sodium formiate quality is 5.776 grams; Catalyzer nickel formate 0.152 gram, phase-transfer catalyst PPG-600 0.38 gram; Mass concentration is 35% sodium formate solution 13.3 grams; Thermo-stabilizer Resorcinol 0.152 gram, antioxidant 4010-NA0.152 gram; Stir; Make above-mentioned raw materials 110 ℃ of reactions 4 hours, lower the temperature after 30 ℃, through ion exchange treatment; Process biomass-based deicing fluid mother liquor, freezing point-70 ℃.
Application implementation example 1: with biomass-based deicing fluid mother liquor preparation deicing fluid
10 kilograms in the biomass-based deicing fluid mother liquor that obtains with embodiment 1-3 stirs to wherein adding each 10-50 gram of rust-preventive agent, inhibiter and defoamer, obtains the deicing fluid product.Performance of products reaches the requirement of China national SH0521-1999 standard fully.
Claims (4)
1. the preparation method of a biomass-based deicing fluid mother liquor is characterized in that, step and condition are following: its prescription is: (1) raw materials of glucose or starch quality are 100 parts; (2) the catalyzer nickel salt is a kind of of nickel acetate, Hydrocerol A nickel, nickel formate or acetylacetonate nickel; The amount of catalyzer is the 0.44-0.80% of raw materials quality; (3) phase-transfer catalyst is PPG-200, PPG-400 or PPG-600; Its consumption is that 1.11-2.00% (4) oxidation inhibitor of raw materials quality is p-NP, thiodiphenylamine or 4010-NA, and consumption is that 0.44-0.80% (5) the auxiliary agent sodium formiate consumption of raw materials quality is the 27.49-30.4% of raw materials quality; By proportioning; The adding mass concentration is 45.0% glucose or amidin in the reaction kettle that has heating temperature control, whipping appts, and mass concentration is 35.0% sodium formate solution, catalyst acetic acid nickel; Phase-transfer catalyst; Add thermo-stabilizer again, antioxidant stirs; Reacted 2-4 hour down at 90-110 ℃; Cool to 30 ℃, after ion-exchange, make a kind of biomass-based deicing fluid mother liquor.
2. the preparation method of a kind of biomass-based deicing fluid mother liquor as claimed in claim 1 is characterized in that, described its prescription is 100 parts for (1) raw materials of glucose quality; (2) the catalyzer nickel salt is a nickel acetate; The amount of catalyzer is 0.44% of a raw materials quality; (3) phase-transfer catalyst is PPG-200, and its consumption is that 1.11% (4) oxidation inhibitor of raw materials quality is p-NP, and consumption is that 0.44% (5) auxiliary agent sodium formiate consumption of raw materials quality is 27.49% of a raw materials quality; Reacted 2 hours down at 105 ℃.
3. the preparation method of a kind of biomass-based deicing fluid mother liquor as claimed in claim 1 is characterized in that, described its prescription is 100 parts for (1) raw starch quality; (2) the catalyzer nickel salt is a Hydrocerol A nickel; The amount of catalyzer is 0.64% of a raw materials quality; (3) phase-transfer catalyst is PPG-400, and its consumption is that 1.49% (4) oxidation inhibitor of raw materials quality is thiodiphenylamine, and consumption is that 0.64% (5) auxiliary agent sodium formiate consumption of raw materials quality is 28.34% of a raw materials quality; Reacted 3 hours down at 90 ℃.
4. the preparation method of a kind of biomass-based deicing fluid mother liquor as claimed in claim 1 is characterized in that, described its prescription is 100 parts for (1) raw starch quality; (2) the catalyzer nickel salt is a nickel formate; The amount of catalyzer is 0.8% of a raw materials quality; (3) phase-transfer catalyst is PPG-600, and its consumption is that 2% (4) oxidation inhibitor of raw materials quality is 4010-NA, and consumption is that 0.8% (5) auxiliary agent sodium formiate consumption of raw materials quality is 30.4% of a raw materials quality; Reacted 4 hours down at 110 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011102302623A CN102352222A (en) | 2011-08-12 | 2011-08-12 | Preparation method of biomass based antifreeze fluid mother liquor |
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| CN2011102302623A CN102352222A (en) | 2011-08-12 | 2011-08-12 | Preparation method of biomass based antifreeze fluid mother liquor |
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| CN102352222A true CN102352222A (en) | 2012-02-15 |
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| CN2011102302623A Pending CN102352222A (en) | 2011-08-12 | 2011-08-12 | Preparation method of biomass based antifreeze fluid mother liquor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111763502A (en) * | 2020-07-23 | 2020-10-13 | 夏莲子 | Automobile antifreeze fluid and preparation method thereof |
| CN113773814A (en) * | 2021-09-24 | 2021-12-10 | 长春工业大学 | Preparation method of bio-based anti-freezing agent |
| WO2024053468A1 (en) * | 2022-09-06 | 2024-03-14 | 日東電工株式会社 | Catalytic reaction method, method for producing organic compound, and catalyst composition |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60166370A (en) * | 1984-02-08 | 1985-08-29 | Takenobu Kondo | Antifreeze water |
| CN1057284A (en) * | 1990-06-09 | 1991-12-25 | 北京铁路局北京科学技术研究所 | Antifreezer for water-bearing particles |
| US5385688A (en) * | 1993-01-08 | 1995-01-31 | American Polywater Corporation | Antifreeze gel composition for use in a cable conduit |
| US20040185066A1 (en) * | 2003-03-17 | 2004-09-23 | Yuh-Jye Uang | Antifreeze gel in a deformable container |
| CN102068021A (en) * | 2009-11-20 | 2011-05-25 | 中国农业科学院蜜蜂研究所 | Preservative for royal jelly and preparation process thereof |
-
2011
- 2011-08-12 CN CN2011102302623A patent/CN102352222A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60166370A (en) * | 1984-02-08 | 1985-08-29 | Takenobu Kondo | Antifreeze water |
| CN1057284A (en) * | 1990-06-09 | 1991-12-25 | 北京铁路局北京科学技术研究所 | Antifreezer for water-bearing particles |
| US5385688A (en) * | 1993-01-08 | 1995-01-31 | American Polywater Corporation | Antifreeze gel composition for use in a cable conduit |
| US20040185066A1 (en) * | 2003-03-17 | 2004-09-23 | Yuh-Jye Uang | Antifreeze gel in a deformable container |
| CN102068021A (en) * | 2009-11-20 | 2011-05-25 | 中国农业科学院蜜蜂研究所 | Preservative for royal jelly and preparation process thereof |
Non-Patent Citations (1)
| Title |
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| 杨湘琼: "《谈谈防冻液》", 《摩托车》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111763502A (en) * | 2020-07-23 | 2020-10-13 | 夏莲子 | Automobile antifreeze fluid and preparation method thereof |
| CN113773814A (en) * | 2021-09-24 | 2021-12-10 | 长春工业大学 | Preparation method of bio-based anti-freezing agent |
| WO2024053468A1 (en) * | 2022-09-06 | 2024-03-14 | 日東電工株式会社 | Catalytic reaction method, method for producing organic compound, and catalyst composition |
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Application publication date: 20120215 |