CN105837304A - Method for manufacturing coated fertilizer based on improved waste oil of sauce residue - Google Patents
Method for manufacturing coated fertilizer based on improved waste oil of sauce residue Download PDFInfo
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- CN105837304A CN105837304A CN201510016894.8A CN201510016894A CN105837304A CN 105837304 A CN105837304 A CN 105837304A CN 201510016894 A CN201510016894 A CN 201510016894A CN 105837304 A CN105837304 A CN 105837304A
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Abstract
The invention belongs to the technical field of environmental science and technology, and belongs to technical fields of a functional polymer and a slow-release fertilizer. Waste oil extracted from sauce residue is subjected to a certain degree of epoxidation modification, and a coated organic-inorganic compound fertilizer having slow release performance is manufactured through an industrial disc pelletizer, so that waste oil is changed into a treasure. As everyone knows, our country has the large production of soy, and the sauce residue is a main by-product from soy manufacture and is abundant in oil content. Particularly, the coarse fat content of the sauce residue taking soybeans as a raw material can reach 25-50% (on a dry basis), some even close to the oil content of peanuts. Waste oil of the sauce residue mainly comprises C16 and C18 triglyceride and many unsaturated double bonds. Through simple treatment and epoxidation of the waste oil of the sauce residue, and through combination with phosphate, the coated organic-inorganic compound fertilizer having slow release performance is manufactured. Therefore, the waste sauce residue is effectively utilized, and a new coated fertilizer material is provided, hoping to offer theoretical exploration and value references for the development of waste oil and the slow-release fertilizer.
Description
Technical field
The invention belongs to technical field of environmental science; and belong to functional polymer and slow release fertilizer technical field; a certain degree of epoxidation modification is carried out by extracting discarded oils and fats from soy sauce residue; and utilizing the principle of industry granulating disc to prepare a kind of organic-inorganic coated compound fertilizer with sustained release performance so that waste grease is turned waste into wealth.
Background technology
China's soy sauce yield is big, and soy sauce residue is the Main By product producing soy sauce, and its oil content is enriched, the most with soybeans as raw materials in soy sauce residue crude fat content up to 25%-50%(butt), some are even close to the oil content of Semen arachidis hypogaeae；Due to history and the difference of dietary habit, producing soy sauce in the world and the country sold is few, the research developing soy sauce residue rarely has report, and for a long time by factors such as technology, market, ideas, the domestic exploitation to soy sauce residue are the rarest.
In China, waste grease is also referred to as " waste oil ", and " hogwash fat " etc., relatively costly due to waste grease recycling, a large amount of waste greases only have small part to be sent to chemical plant to make fatty acid and soap.In recent years, government strengthens and perfects waste in-ore rate management legal system and specification, and the research on utilization utilizing waste in-ore rate to produce the new forms of energy such as biodiesel becomes focus；But owing to waste in-ore rate free fatty acid content is high, and degree difference of becoming sour is very big, is used for producing biodiesel and yet suffers from some technical barriers.Waste oil rarely has report at the applied research of agriculture field, rarely found as coating controlled-release fertilizer film material raw material.
Often will the most not only cause the waste of resource along with rain water runoff or distillation itself, Soil structure also can be caused to destroy before crop not yet utilizes after common incorporation of fertilizerin the soil, the negative consequence such as water source eutrophication.In order to improve utilization rate of fertilizer, preventing the pollution of the environment, promote the sustainable development of agricultural, research and extension has utilization rate slow release fertilizer high, environment amenable, has highly important economic worth and long-range practical guided significance.Although current release-controlled coated fertilizer is worldwide achieved with bigger development, but owing to commercially available price is 3-8 times of common fertilizer, significantly limit its popularization and application, therefore the new and effective cheap release-controlled coated material of developmental research is the key of solution problem.Soy sauce residue waste oil is mainly C16And C18 Triglyceride, and containing more conjugated double bond, be prepared as release-controlled coated material by the epoxidation modification under certain condition, it is not necessary to special solvent and high-temperature high-pressure apparatus can be in fertilizer surface polyreaction film forming.
Summary of the invention
The target of the present invention; by extracting waste oil from discarded soy sauce residue, and carry out waste oil epoxidation modification, utilize the principle of industry granulating disc; prepare the coat fertilizer with certain sustained release performance in conjunction with ground phosphate rock and homemade firming agent, make the production cost of coat fertilizer be greatly lowered.For completing foregoing invention purpose, the present invention includes that following steps is rapid:
1) discarded soy sauce residue is collected from soy sauce factory, first in convection oven 100 DEG C soy sauce residue is dried 1 h, then the squeezing of oils and fats is carried out at small oil press (6YL-30 household type), finally filter off residual foreign material the purest i.e. available soy sauce residue waste oil with sieves, or rectification again after extracting with organic solvent such as acetone etc..
2) weigh and join in the there-necked flask of 100ml from the crude fat 20-30g extracted from soy sauce residue, it is heated to uniform temperature (50-60 DEG C) and is initially added into epoxidizing agent (acetic acid, hydrogen peroxide and concentrated sulphuric acid configure by a certain percentage), mixing speed is generally 20r/s, simultaneously by supersound process, rate of addition is uniform before and after wanting, after reaction 3-5h, static layering, first dividing sub-cloud waste liquid, oil reservoir is first slightly washed till about pH=5.0 with diluted alkaline, then is washed till pH=7.0 with saturated tap water.Then decompression distillation obtains epoxidation waste oil.
3) the epoxidation waste oil produced is poured into sealing in glass flask in air dry oven after high temperature (180-200 DEG C) pre-polymerization 1-2h to save backup.
4) a certain amount of carbamide 10.0-20.0g and ground phosphate rock 5.0-10.0g is weighed; utilize the principle of granulating disc; first by the conical flask pouring rapidly 250ml after carbamide hot air drying 5 min into; then drip homemade modified soy sauce residue waste oil 2-3 to drip; rocking-turn 1-2min in the case of with manual rotation as 3-6r/s; being slowly added into 1-2g ground phosphate rock rocking-turn 5min, rotating speed is 2-5r/s；Add modified soy sauce residue waste oil 2-3 to drip and rocking-turn 2-5min, be slowly added into 1-2g ground phosphate rock rocking-turn 5min, rotating speed 3-5r/s；So repeating 5-8 time, finally add a droplet modification soy sauce residue waste oil and homemade firming agent uniform rocking-turn 5 min, so modified soy sauce residue waste oil aliphatic radical coat fertilizer just prepares.
5) the above-mentioned coat fertilizer prepared is poured into surface plate, 40-50h in the air dry oven of 40-60 DEG C, it is then placed in sealing in bag, and preserves in the environment being relatively dried.
Detailed description of the invention:
Below by concrete example, the present invention is further illustrated.
Embodiment one,
Weigh and join in the there-necked flask of 100ml from the crude fat 30g extracted from soy sauce residue, it is heated to uniform temperature (50-60 DEG C) and is initially added into epoxidizing agent (acetic acid 10.8g, hydrogen peroxide 29.2g and concentrated sulphuric acid 0.02ml), mixing speed is generally 20r/s, supersound process simultaneously, rate of addition is uniform before and after wanting, after reaction 5h, static layering, first dividing sub-cloud waste liquid, oil reservoir is first slightly washed till about pH=5 with diluted alkaline, then is washed till pH=7.0 with saturated tap water；Then decompression distillation obtains epoxidation waste oil；Again the epoxidation waste oil produced is poured into after high temperature (180 DEG C) pre-polymerization 1-2h to seal in glass flask in air dry oven and save backup.Recording epoxide number is 2.56.
Weigh a certain amount of carbamide 10.0g and ground phosphate rock 5.0g, first by the conical flask pouring rapidly 250ml after carbamide hot air drying 5 min into, then drip homemade modified soy sauce residue waste oil 2-5 to drip, rocking-turn 2min in the case of with manual rotation as 3-5r/s, being slowly added into 1g ground phosphate rock rocking-turn 5min, rotating speed is 2-5r/s；Add 2-5 and drip modified soy sauce residue waste oil rocking-turn 2min, be slowly added into 1g ground phosphate rock rocking-turn 5min, rotating speed 3-5r/s；So repeat 3-5 time by above-mentioned steps, finally drip a droplet modification soy sauce residue waste oil and homemade firming agent at the uniform velocity rocking-turn 5 min, the coat fertilizer prepared is poured into surface plate in the air dry oven of 40-60 DEG C, after 40-50h, seals room temperature preservation.
Embodiment two,
Weigh and join in the there-necked flask of 100ml from the crude fat 30g extracted from soy sauce residue, it is heated to uniform temperature (50-60 DEG C) and is initially added into epoxidizing agent (acetic acid 8.5g, hydrogen peroxide 31.5g and concentrated sulphuric acid 0.02ml), mixing speed is generally 20r/s, supersound process simultaneously, rate of addition is uniform before and after wanting, after reaction 5h, static layering, first dividing sub-cloud waste liquid, oil reservoir is first slightly washed till about pH=5 with diluted alkaline, then is washed till pH=7.0 with saturated tap water；Then decompression distillation obtains epoxidation waste oil；Again the epoxidation waste oil produced is poured into after high temperature (180 DEG C) pre-polymerization 1-2h to seal in glass flask in air dry oven and save backup.Recording epoxide number is 3.62.
Weigh a certain amount of carbamide 10.0g and ground phosphate rock 5.0g, first by the conical flask pouring rapidly 250ml after carbamide hot air drying 5 min into, then drip homemade modified soy sauce residue waste oil 2-5 to drip, rocking-turn 2min in the case of with manual rotation as 3-5r/s, being slowly added into 1g ground phosphate rock rocking-turn 5min, rotating speed is 2-5r/s；Add 2-5 and drip modified soy sauce residue waste oil rocking-turn 2min, be slowly added into 1g ground phosphate rock rocking-turn 5min, rotating speed 3-5r/s；So repeat 3-5 time by above-mentioned steps, finally drip a droplet modification soy sauce residue waste oil and homemade firming agent rocking-turn 5 min, the coat fertilizer prepared is poured into surface plate in the air dry oven of 40-60 DEG C, after 40-50 h, seals room temperature preservation.
Embodiment three,
Weigh and join in the there-necked flask of 100ml from the crude fat 30g extracted from soy sauce residue, it is heated to uniform temperature (50-60 DEG C) and is initially added into epoxidizing agent (acetic acid 6.0g, hydrogen peroxide 34g and concentrated sulphuric acid 0.04ml), mixing speed is generally 20r/s, supersound process simultaneously, rate of addition is uniform before and after wanting, after reaction 5h, static layering, first dividing sub-cloud waste liquid, oil reservoir is first slightly washed till about pH=5 with diluted alkaline, then is washed till pH=7.0 with saturated tap water；Then decompression distillation obtains epoxidation waste oil；Again the epoxidation waste oil produced is poured into after high temperature (190 DEG C) pre-polymerization 1-2h to seal in glass flask in air dry oven and save backup.Recording epoxide number is 4.57.
Weigh a certain amount of carbamide 10.0g and ground phosphate rock 5.0g, first by the conical flask pouring rapidly 250ml after carbamide hot air drying 5 min into, then drip homemade modified soy sauce residue waste oil 2-5 to drip, rocking-turn 2min in the case of with manual rotation as 3-5r/s, being slowly added into 1g ground phosphate rock rocking-turn 5min, rotating speed is 2-5r/s；Add 2-5 and drip modified soy sauce residue waste oil rocking-turn 5min, be slowly added into 1g ground phosphate rock rocking-turn 5min, rotating speed 3-5r/s；So repeat 3-5 time by above-mentioned steps, finally drip a droplet modification soy sauce residue waste oil and homemade firming agent rocking-turn 5 min, the coat fertilizer prepared is poured into surface plate in the air dry oven of 40-60 DEG C, after 40-50 h, seals room temperature preservation.
Embodiment four,
Weigh and join in the there-necked flask of 100ml from the crude fat 30g extracted from soy sauce residue, it is heated to uniform temperature (50-60 DEG C) and is initially added into epoxidizing agent (acetic acid 6.0g, hydrogen peroxide 34g and concentrated sulphuric acid 0.06ml), mixing speed is generally 20r/s, supersound process simultaneously, rate of addition is uniform before and after wanting, after reaction 5h, static layering, first dividing sub-cloud waste liquid, oil reservoir is first slightly washed till about pH=5 with diluted alkaline, then is washed till pH=7.0 with saturated tap water；Then decompression distillation obtains epoxidation waste oil；Again the epoxidation waste oil produced is poured into after high temperature (180 DEG C) pre-polymerization 1-2h to seal in glass flask in air dry oven and save backup.Recording epoxide number is 4.99.
Weigh a certain amount of carbamide 10.0g and ground phosphate rock 5.0g, first by the conical flask pouring rapidly 250ml after carbamide hot air drying 5 min into, then drip homemade modified soy sauce residue waste oil 2-5 to drip, rocking-turn 2min in the case of with manual rotation as 3-5r/s, being slowly added into 1g ground phosphate rock rocking-turn 5min, rotating speed is 2-5r/s；Add 2-5 and drip modified soy sauce residue waste oil rocking-turn 2min, be slowly added into 1g ground phosphate rock rocking-turn 5min, rotating speed 3-5r/s；So repeat 3-5 time by above-mentioned steps, finally drip a droplet modification soy sauce residue waste oil and homemade firming agent rocking-turn 5 min, the coat fertilizer prepared is poured into surface plate in the air dry oven of 40-60 DEG C, after 30-50 h, seals room temperature preservation.Recording initial stage nutrient release rate by hydrostatic method is 13.9%, and it is 75.6% that 28d adds up release rate, basically reaches the standard of slow-release fertilizer.
Embodiment five,
Weigh and join in the there-necked flask of 100ml from the crude fat 30g extracted from soy sauce residue, it is heated to uniform temperature (50-60 DEG C) and is initially added into epoxidizing agent (acetic acid 6.0g, hydrogen peroxide 34g and concentrated sulphuric acid 0.08ml), mixing speed is generally 20r/s, supersound process simultaneously, rate of addition is uniform before and after wanting, after reaction 5h, static layering, first dividing sub-cloud waste liquid, oil reservoir is first slightly washed till about pH=5 with diluted alkaline, then is washed till pH=7.0 with saturated tap water；Then decompression distillation obtains epoxidation waste oil；Again the epoxidation waste oil produced is poured into after high temperature (180 DEG C) pre-polymerization 1-2h to seal in glass flask in air dry oven and save backup.Recording epoxide number is 5.22.
Weigh a certain amount of carbamide 10.0g and ground phosphate rock 5.0g, first by the conical flask pouring rapidly 250ml after carbamide hot air drying 5 min into, then drip homemade modified soy sauce residue waste oil 2-5 to drip, rocking-turn 2min in the case of with manual rotation as 3-5r/s, being slowly added into 1g ground phosphate rock rocking-turn 5min, rotating speed is 2-5r/s；Add 2-5 and drip modified soy sauce residue waste oil rocking-turn 2min, be slowly added into 1g ground phosphate rock rocking-turn 5min, rotating speed 3-5r/s；So repeat 3-5 time by above-mentioned steps, finally drip a droplet modification soy sauce residue waste oil and homemade firming agent rocking-turn 5 min, the coat fertilizer prepared is poured into surface plate in the air dry oven of 40-60 DEG C, after 30-40 h, seals room temperature preservation.Recording initial stage nutrient release rate by hydrostatic method is 11.6%, and it is 74.8% that 28d adds up release rate, basically reaches the standard of release-controlled coated fertilizer.
Claims (9)
1. the preparation method of a modified soy sauce residue waste oil aliphatic radical coat fertilizer, it is characterised in that.
2. the method includes that following steps is rapid:
The preparation of epoxidation waste oil: collect discarded soy sauce residue from soy sauce factory, first in convection oven 100 DEG C soy sauce residue is dried 1 h, the squeezing of oils and fats is carried out at small oil press (6YL-30 household type), typically can squeeze 2-3 time continuously, filter off residual foreign material the purest i.e. available soy sauce residue waste oil with sieves, or with after organic solvent such as acetone extract again rectification extract and also can get purer waste oil；Then weigh and join in the there-necked flask of 100ml from the crude fat 20-30g extracted from soy sauce residue, it is heated to uniform temperature (50-60 DEG C) and is initially added into epoxidizing agent (acetic acid, hydrogen peroxide and concentrated sulphuric acid configure by a certain percentage), mixing speed is generally 20r/s, supersound process simultaneously, rate of addition is uniform before and after wanting, after reaction 3-5h, static layering, first dividing sub-cloud waste liquid, oil reservoir is first slightly washed till about pH=5 with diluted alkaline, then is washed till pH=7.0 with saturated tap water；Decompression distillation i.e. obtains epoxidation waste oil, the epoxidation waste oil produced is poured into sealing in glass flask in air dry oven save backup after high temperature pre-polymerization 1-2h.
3. the preparation of coat fertilizer: weigh a certain amount of carbamide 10.0-20.0g and ground phosphate rock 5.0-10.0g; utilize the principle of granulating disc; first by the conical flask pouring rapidly 250ml after carbamide hot air drying 5-10min into; then drip homemade modified soy sauce residue waste oil 2-3 to drip; rocking-turn 1-2min in the case of with manual rotation as 3-6r/s; being slowly added into 1-2g ground phosphate rock rocking-turn 5min, rotating speed is 2-5r/s；Add modified soy sauce residue waste oil 2-3 and drip modified soy sauce residue waste oil rocking-turn 2-5min, be slowly added into 1-2g ground phosphate rock rocking-turn 5min, rotating speed 3-5r/s；So repeating 5-8 time, finally add a droplet modification soy sauce residue waste oil and homemade firming agent rocking-turn 5 min, so modified soy sauce residue waste oil aliphatic radical coat fertilizer just prepares；The above-mentioned coat fertilizer prepared is poured into surface plate, 30-50 h in the air dry oven of 40-60 DEG C, it is then placed in sealing in bag, and preserves in the environment being relatively dried.
The preparation method of a kind of modified soy sauce residue waste oil aliphatic radical coat fertilizer the most as claimed in claim 2, it is characterised in that waste oil can first be conjugated modified epoxidation again, and in waste oil epoxidation preparation process, supersound process effect is preferable, model of action 5s/7s.
The preparation method of a kind of modified soy sauce residue waste oil aliphatic radical coat fertilizer the most as claimed in claim 2, it is characterised in that after waste oil epoxidation can high temperature pre-polymerization 1-2h, optimum temperature 180-220 DEG C, or compound with homemade adhesion agent.
The preparation method of a kind of modified soy sauce residue waste oil aliphatic radical coat fertilizer the most as claimed in claim 2, it is characterised in that in the case of reaction waste oil takes 30g, the optimum proportioning of epoxidizing agent is acetic acid: hydrogen peroxide=7.0:33.0, concentrated sulphuric acid 0.08ml.
The preparation method of a kind of modified soy sauce residue waste oil aliphatic radical coat fertilizer the most as claimed in claim 2, it is characterised in that the optimal reaction temperature of modified epoxy waste oil is 80 DEG C, and optimum reacting time is 4-5 h.
The preparation method of a kind of modified soy sauce residue waste oil aliphatic radical coat fertilizer the most as claimed in claim 3, it is characterised in that the optimised process of peplos be nitrogenous fertilizer, ground phosphate rock ratio be 1:0.5, the Best Times of peplos is 30-40min, optimal number of times 5-8 time.
The preparation method of a kind of modified soy sauce residue waste oil aliphatic radical coat fertilizer the most as claimed in claim 3, it is characterised in that the optimum temperature solidifying preservation after peplos is 40-60 DEG C, and the time is 30-50h.
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| CN107459435A (en) * | 2017-09-22 | 2017-12-12 | 芜湖晋诚农业科技有限公司 | A kind of fertilizer for improving tomato quality |
| CN107459436A (en) * | 2017-09-22 | 2017-12-12 | 芜湖晋诚农业科技有限公司 | A kind of fertilizer of anti-tomato continuous cropping disease |
| CN108821846A (en) * | 2018-06-01 | 2018-11-16 | 山东农业大学 | A kind of high molecular slow-release fertilizer using gutter oil synthesis |
| CN109336670A (en) * | 2018-10-08 | 2019-02-15 | 仲恺农业工程学院 | A kind of method and its application of oil modification |
| CN109699440A (en) * | 2019-03-06 | 2019-05-03 | 陈硕 | A kind of multifunctional ecological seedling culturing substrate block |
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- 2015-01-14 CN CN201510016894.8A patent/CN105837304A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107459435A (en) * | 2017-09-22 | 2017-12-12 | 芜湖晋诚农业科技有限公司 | A kind of fertilizer for improving tomato quality |
| CN107459436A (en) * | 2017-09-22 | 2017-12-12 | 芜湖晋诚农业科技有限公司 | A kind of fertilizer of anti-tomato continuous cropping disease |
| CN108821846A (en) * | 2018-06-01 | 2018-11-16 | 山东农业大学 | A kind of high molecular slow-release fertilizer using gutter oil synthesis |
| CN109336670A (en) * | 2018-10-08 | 2019-02-15 | 仲恺农业工程学院 | A kind of method and its application of oil modification |
| CN109336670B (en) * | 2018-10-08 | 2021-07-27 | 仲恺农业工程学院 | Method for modifying grease and application thereof |
| CN109699440A (en) * | 2019-03-06 | 2019-05-03 | 陈硕 | A kind of multifunctional ecological seedling culturing substrate block |
| CN109699440B (en) * | 2019-03-06 | 2021-12-28 | 陈硕 | Multifunctional ecological seedling raising substrate block |
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