CN107417329A - A kind of method that plant asphalt extraction triacontanol prepares fertilizer - Google Patents
A kind of method that plant asphalt extraction triacontanol prepares fertilizer Download PDFInfo
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- CN107417329A CN107417329A CN201710663158.0A CN201710663158A CN107417329A CN 107417329 A CN107417329 A CN 107417329A CN 201710663158 A CN201710663158 A CN 201710663158A CN 107417329 A CN107417329 A CN 107417329A
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- China
- Prior art keywords
- plant asphalt
- triacontanol
- prepares fertilizer
- urea
- asphalt extraction
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C9/00—Fertilisers containing urea or urea compounds
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G5/00—Fertilisers characterised by their form
- C05G5/20—Liquid fertilisers
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Fertilizers (AREA)
Abstract
The present invention relates to the method that a kind of plant asphalt extraction triacontanol prepares fertilizer, comprise the following steps：1) ester exchange reaction is carried out under plant asphalt basic conditions；2) cool, diaphragm filter press filters to obtain filter cake；3) filter cake adds n-hexane dissolution, separates to obtain clear liquid；4) step 3) clear liquid adds proper amount of acetone, gradient cooling, collects crystal；5) dissolution of crystals adds urea to stir to dissolving, cooling and collects urea crystal in hot ethanol；6) urea crystal is dissolved in the aqueous solution, compounds other active materials, filling to produce crop nutrient solution.This technique extracts concentrated active ingredients using crystallization mode twice from plant asphalt, compounds other materials, can remarkably promote plant growth, improves resistance, has major application value.
Description
Technical field
The present invention relates to a kind of preparation method of the crop nutrient solution from plant asphalt higher aliphatic, belongs to fertilizer life
Produce technical field.
Background technology
Plant asphalt is also known as black pin, is the leftover bits and pieces remained in aliphatic acid, oleic acid or fatty acid methyl ester production process.When
Preceding fatty acid methyl ester is as " biodiesel " a large amount of productions in the world, and this creates the terminal substantial amounts of plant asphalt.Due to planting
Thing pitch obtains by high temperature distillation technique, and viscosity is big, color and luster is deep, ash content is high, flash-point is high, traditional using plant asphalt as pot
The method of stove fuel easily causes the coking of boiler, declines boiler thermal output, the serious service life for reducing boiler.Therefore
Exploitation plant asphalt new application is significant.
With reference to plant asphalt substance characteristics, extraction high value added product is research and development focus in recent years.Patent
CN201310671990.7 discloses a kind of method that fatty acid methyl ester is extracted from plant asphalt, by being esterified, centrifuging,
Alkali is adjusted, and obtains fatty acid methyl ester product；Patent CN202509040U discloses a kind of plant asphalt, and rectifying prepares fatty acid methyl again
Ester apparatus, the device ensure that material fluidity is good in distillation process again, it is not easy to block heater；Patent
CN200810020358.5, CN201510467244.5 are related to the method that phytosterol is extracted from plant asphalt, through high pressure ester
Change, be evaporated under reduced pressure and remove fatty acid ester, then thick sterol is obtained by solvent extraction or method for saponification, through the work such as decolourizing, recrystallizing
Skill produces finished product.Report that plant asphalt Land use systems are concentrated mainly on the extraction separation of fatty acid methyl ester and phytosterol
On, preparation and utilization to higher aliphatic have no report.
Higher aliphatic especially triacontanol is a kind of wide spectrum, efficient, new plant growth regulator, can be promoted
Crop germinates, taken root, the growth of cauline leaf and blooms, and strengthens photosynthesis, improves setting percentage, drought resisting, cold tolerance, increases yield
Deng.Patent CN03113007.0 is using chaff wax as raw material, using ultrasound hydrolysis rice bran wax, molecular distillation technique separation 28
Alkanol, triacontanol, the product that purity is more than 80% is prepared；Patent CN201210280127.4 by calcium oxide at high temperature
React, then extracted with ethanol, pillar molecular distillation with natural animal wax, collect the fraction that temperature is 200-215 DEG C, obtain high-purity
Spend triacontanol.Patent CN201410482434.X discloses a kind of microwave, solid super base catalysis method carries from natural beeswax
The technique for taking triacontanol.Above-mentioned triacontanol preparation method is directed to the technologies such as ultrasound, molecular distillation, microwave, is produced into
This height, limit triacontanol large-scale production and use.
The content of the invention
It is contemplated that design a kind of method that plant asphalt extraction triacontanol prepares fertilizer, it is characterised in that including
Following steps：
1) 100 parts of plant asphalt, 10 parts of alcohol sodium solution, 10 parts of methanol are well mixed, 45-50 DEG C of maintenance reaction temperature, stir
Mix 2-3h；
2) step 1) reaction solution is very fast is cooled to less than 5 DEG C, and diaphragm filter press filters to obtain filter cake, and filtration cakes torrefaction weightlessness does not surpass
Cross 6%；
3) filter cake adds 8-10 times of volume n-hexane dissolution, and supernatant liquor is separated to obtain in extractor；
4) step 3) clear liquid adds proper amount of acetone, and gradient cooling stops stirring and maintain temperature 8-10h, filter to obtain crude product to 5 DEG C
Crystallization；
5) step 4) dissolution of crystals adds appropriate urea to stir to dissolving, gradient cooling and stops stirring to 7 DEG C in hot ethanol
Mix and maintain temperature 2-3h, filter to obtain urea crystal；
6) step 5) urea crystal is dissolved in 5 times of v aqueous solutions, built amino-acid 5%-8%, alginic acid 0.5%-
1%th, low-molecular weight chitoglycan 2%-3%, it is filling to produce crop nutrient solution.
Further, step 1) sodium alkoxide solution manufacturing method is that methanol solution 100ml is hydrogenated with sodium oxide molybdena 20g, controls temperature 60
DEG C -70 DEG C, stirring is to being completely dissolved.
Further, step 2) temperature fall time is no more than 2h.
Further, step 4) acetone dosage is the 1/3 of hexane solution volume.
Further, step 4) gradient cooling speed is 10 DEG C/h.
Further, step 5) amount of urea is 2 times of crude crystalline.
Further, step 5) gradient cooling speed is 5 DEG C/h.
Further, the step 6) amino acid is one or more of mixing of tryptophan, aspartic acid, phenylalanine.
The crop nutrient solution for the active material containing plant asphalt being prepared using the above method is also claimed in the present invention
And its application in apple, grape, wheat, corn, Kiwi berry, tomato, potatoes and other crops.
The beneficial effects of the invention are as follows：
1) higher aliphatic in plant asphalt is prepared first, bioactivity is high, promotees crop production positive effect.Plant
The middle-and-high-ranking fatty alcohol composition of thing pitch is significantly different with animal wax and rice bran wax, and octacosane alcohol content is low, and purifying is more convenient, raw
Thing activity is high.
2) present invention prepares simple production process, and equipment requirement is low, is easy to large-scale production.By crystallization processes twice,
Extraction, concentrated cost are reduced, is adapted to batch production.
3) raw material sources enrich.The present invention is fats and oils processing leftover bits and pieces using material plant pitch, and deposit enriches and price
It is cheap, it is natural harmless, it is preferable raw material.
Embodiment
The principle and feature of the present invention are described below in conjunction with example, the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the present invention.
The preparation of alcohol sodium solution：Methanol solution 1000L is hydrogenated with sodium oxide molybdena 200kg, controls -70 DEG C of temperature 60 C, stirring is extremely
It is completely dissolved.
Embodiment 1
1) plant asphalt 500L, alcohol sodium solution 50L, methanol 50L are well mixed, 45-50 DEG C of maintenance reaction temperature, stirring
3h；
2) step 1) reaction solution is very fast is cooled to less than 5 DEG C, and temperature fall time is no more than 2 hours, and diaphragm filter press filters
Filter cake, filtration cakes torrefaction is weightless to be no more than 6%, and filter cake nearly weighs 158kg；
3) filter cake adds 8 times of volume n-hexane dissolutions, and supernatant liquor about 1100L is separated to obtain in extractor；
4) step 3) clear liquid adds 366L acetone, and for gradient cooling to 5 DEG C, rate of temperature fall is 10 DEG C/h, stops stirring and maintains temperature
10h is spent, filters to obtain crude crystalline 31kg；
5) step 4) dissolution of crystals adds 62kg urea to stir to dissolving in hot ethanol, and gradient cooling is to 7 DEG C, cooling speed
Rate is 5 DEG C/h, stops stirring and maintains temperature 3h, filters to obtain urea crystal 72kg；
6) step 5) urea crystal is dissolved in 5 times of v aqueous solutions, compounding tryptophan 5%, alginic acid 0.5%, low point
Son amount chitosan 2%, it is filling to produce crop nutrient solution 360L.
7) gained crop nutrient solution dilutes 200 times and sprayed in vine, and fruit expanding period sprays 2 times, every minor tick 12 days.
It is dry crude strong that grape branch can be obtained, blade is stood upright, and fruit head is rectified full, and yield increased.
Embodiment 2
1) plant asphalt 2000L, alcohol sodium solution 200L, methanol 200L are well mixed, and 45-50 DEG C of maintenance reaction temperature, are stirred
Mix 3h；
2) step 1) reaction solution is very fast is cooled to less than 5 DEG C, and temperature fall time is no more than 2 hours, and diaphragm filter press filters
Filter cake, filtration cakes torrefaction is weightless to be no more than 6%, and filter cake nearly weighs 705kg；
3) filter cake adds 8 times of volume n-hexane dissolutions, and supernatant liquor about 5600L is separated to obtain in extractor；
4) step 3) clear liquid adds 1800L acetone, and for gradient cooling to 5 DEG C, rate of temperature fall is 10 DEG C/h, stops stirring and maintains temperature
10h is spent, filters to obtain crude crystalline 140kg；
5) step 4) dissolution of crystals adds 280kg urea to stir to dissolving in hot ethanol, and gradient cooling is to 7 DEG C, cooling speed
Rate is 5 DEG C/h, stops stirring and maintains temperature 3h, filters to obtain urea crystal 320kg；
6) step 5) urea crystal is dissolved in 5 times of v aqueous solutions, compounding phenylalanine 8%, alginic acid 0.6%, low
Molecular weight chitosan 2%, it is filling to produce crop nutrient solution 1600L.
7) by the dilution of crop nutrient solution 100 times spray in apple tree fruit expanding period 3 times, per minor tick 10 days.Reality can be obtained
It is vigorous to test group fruit tree growing way, resistance enhancing, fruit is rectified, and high quality fruit rate improves.
Embodiment 3
1) plant asphalt 1000L, alcohol sodium solution 100L, methanol 100L are well mixed, and 45-50 DEG C of maintenance reaction temperature, are stirred
Mix 3h；
2) step 1) reaction solution is very fast is cooled to less than 5 DEG C, and temperature fall time is no more than 2 hours, and diaphragm filter press filters
Filter cake, filtration cakes torrefaction is weightless to be no more than 6%, and filter cake nearly weighs 350kg；
3) filter cake adds 8 times of volume n-hexane dissolutions, and supernatant liquor about 2800L is separated to obtain in extractor；
4) step 3) clear liquid adds 930L acetone, and for gradient cooling to 5 DEG C, rate of temperature fall is 10 DEG C/h, stops stirring and maintains temperature
10h is spent, filters to obtain crude crystalline 70kg；
5) step 4) dissolution of crystals adds 140kg urea to stir to dissolving in hot ethanol, and gradient cooling is to 7 DEG C, cooling speed
Rate is 5 DEG C/h, stops stirring and maintains temperature 3h, filters to obtain urea crystal 163kg；
6) step 5) urea crystal is dissolved in 5 times of v aqueous solutions, compounding aspartic acid 3%, tryptophan 5%, marine alga
Acid 0.8%, low-molecular weight chitoglycan 3%, it is filling to produce crop nutrient solution 820L.
7) crop nutrient solution dilutes 150 times of foliage-sprays in tomato fruit expanding stage, every minor tick 10 days, sprays 2 altogether
It is secondary, can obtain experimental group compared to control tree vigo(u)r it is vigorous, blade is dense to stand upright, fruit individual rectify it is full, malformed fruit significantly reduces, production
Amount lifting.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc., it should be included in the scope of the protection.
Claims (9)
1. a kind of method that plant asphalt extraction triacontanol prepares fertilizer, it is characterised in that comprise the following steps：
1) 100 parts of plant asphalt, 10 parts of alcohol sodium solution, 10 parts of methanol are well mixed, 45-50 DEG C of maintenance reaction temperature, stir 2-
3h；
2) step 1) reaction solution is very fast is cooled to less than 5 DEG C, and diaphragm filter press filters to obtain filter cake, and filtration cakes torrefaction weightlessness is no more than
6%；
3) filter cake adds 8-10 times of volume n-hexane dissolution, and supernatant liquor is separated to obtain in extractor；
4) step 3) clear liquid adds proper amount of acetone, and gradient cooling stops stirring and maintain temperature 8-10h, filter to obtain crude product knot to 5 DEG C
It is brilliant；
5) step 4) dissolution of crystals adds appropriate urea to stir to dissolving in hot ethanol, and gradient cooling stops stirring dimension to 7 DEG C
Temperature 2-3h is held, filters to obtain urea crystal；
6) step 5) urea crystal is dissolved in 5 times of v aqueous solutions, built amino-acid 5%-8%, alginic acid 0.5%-1%,
Low-molecular weight chitoglycan 2%-3%, it is filling to produce crop nutrient solution.
2. the method that a kind of plant asphalt extraction triacontanol according to claim 1 prepares fertilizer, it is characterised in that step
Rapid 1) sodium alkoxide solution manufacturing method is that methanol solution 100ml is hydrogenated with sodium oxide molybdena 20g, controls -70 DEG C of temperature 60 C, stirs to complete
Dissolving.
3. the method that a kind of plant asphalt extraction triacontanol according to claim 1 prepares fertilizer, it is characterised in that step
Rapid 2) temperature fall time is no more than 2h.
4. the method that a kind of plant asphalt extraction triacontanol according to claim 1 prepares fertilizer, it is characterised in that step
Rapid 4) acetone dosage is the 1/3 of hexane solution volume.
5. the method that a kind of plant asphalt extraction triacontanol according to claim 1 prepares fertilizer, it is characterised in that step
Rapid 4) gradient cooling speed is 10 DEG C/h.
6. the method that a kind of plant asphalt extraction triacontanol according to claim 1 prepares fertilizer, it is characterised in that step
Rapid 5) amount of urea is 2 times of crude crystalline.
7. the method that a kind of plant asphalt extraction triacontanol according to claim 1 prepares fertilizer, it is characterised in that step
Rapid 5) gradient cooling speed is 5 DEG C/h.
8. the method that a kind of plant asphalt extraction triacontanol according to claim 1 prepares fertilizer, it is characterised in that step
Rapid 6) described amino acid is one or more of mixing of tryptophan, aspartic acid, phenylalanine.
9. the active material containing plant asphalt that a kind of preparation method according to any one of claim 1-8 is prepared
Crop nutrient solution and its application in apple, grape, wheat, corn, Kiwi berry, tomato, potatoes and other crops.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710663158.0A CN107417329A (en) | 2017-08-05 | 2017-08-05 | A kind of method that plant asphalt extraction triacontanol prepares fertilizer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710663158.0A CN107417329A (en) | 2017-08-05 | 2017-08-05 | A kind of method that plant asphalt extraction triacontanol prepares fertilizer |
Publications (1)
| Publication Number | Publication Date |
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| CN107417329A true CN107417329A (en) | 2017-12-01 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201710663158.0A Withdrawn CN107417329A (en) | 2017-08-05 | 2017-08-05 | A kind of method that plant asphalt extraction triacontanol prepares fertilizer |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109942369A (en) * | 2019-04-15 | 2019-06-28 | 山东新元素生物科技有限公司 | The method of long-chain fatty alcohol is extracted from vitamin E production residual oil |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03178901A (en) * | 1989-12-06 | 1991-08-02 | Teijin Ltd | Method for improving taste of rice grain |
| CN1522239A (en) * | 2001-04-27 | 2004-08-18 | 豪泽公司 | High molecular weight primary aliphatic alcohols obtained from natural products and uses thereof |
| CN103666769A (en) * | 2013-12-10 | 2014-03-26 | 浙江嘉澳环保科技股份有限公司 | Method for extracting fatty acid methyl ester from vegetable pitch |
| CN105001297A (en) * | 2015-08-03 | 2015-10-28 | 刘火成 | Method for extracting phytosterol from plant pitch |
| CN106007843A (en) * | 2016-05-17 | 2016-10-12 | 烟台固特丽生物科技股份有限公司 | Method for producing water-soluble trace element fertilizer by embedding method |
-
2017
- 2017-08-05 CN CN201710663158.0A patent/CN107417329A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03178901A (en) * | 1989-12-06 | 1991-08-02 | Teijin Ltd | Method for improving taste of rice grain |
| CN1522239A (en) * | 2001-04-27 | 2004-08-18 | 豪泽公司 | High molecular weight primary aliphatic alcohols obtained from natural products and uses thereof |
| CN103666769A (en) * | 2013-12-10 | 2014-03-26 | 浙江嘉澳环保科技股份有限公司 | Method for extracting fatty acid methyl ester from vegetable pitch |
| CN105001297A (en) * | 2015-08-03 | 2015-10-28 | 刘火成 | Method for extracting phytosterol from plant pitch |
| CN106007843A (en) * | 2016-05-17 | 2016-10-12 | 烟台固特丽生物科技股份有限公司 | Method for producing water-soluble trace element fertilizer by embedding method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109942369A (en) * | 2019-04-15 | 2019-06-28 | 山东新元素生物科技有限公司 | The method of long-chain fatty alcohol is extracted from vitamin E production residual oil |
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Application publication date: 20171201 |