CN103451009B - Preparation method of non-edible animal and plant crude oil refined oil - Google Patents
Preparation method of non-edible animal and plant crude oil refined oil Download PDFInfo
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Abstract
The invention relates to a preparation method of a non-edible animal and plant crude oil refined oil. The method includes: filtering squeezed or extracted crude oil, removing solid particle impurities, conducting heating to 40-80DEG C; under stirring, adding a conversion-complexing agent accounting for 1-3% of the mass of the crude oil, conducting constant temperature stirring for 50-90min, employing centrifugal separation at the end of reaction to obtain degummed oil and oil saponins; dehydrating the degummed oil under a vacuum degree of 0.07-0.09MPa and a temperature of 95-105DEG C for 15-25min, heating the dehydrated oil to 90-110DEG C, adding 1-4% of an adsorbent, performing constant temperature stirring for 10-30min, and conducting filtering to obtain the refined oil. While removing phosphorus, metals and other impurities efficiently, the method maintains the acid value of the oil constant, thereby reducing loss and improving the refined oil yield. The method has the characteristics of simple process, low energy consumption, no wastewater discharge, and high stability, etc.
Description
Invention field
The invention belongs to the processing category of animal-plant oil, particularly relate to the preparation method of the refining oil of the raw plant oil, waste grease and the algae grease that squeeze or extract.
Background technology
Along with the development of world economy, the increase day by day of petroleum resources consumption, energy shortage has become the significant problem affecting human society sustainable development.Consider for national energy security, renewable energy source is competitively sought to alleviate the nervous problem of oil in countries in the world.Bioenergy is due to rich reserves, and there is environmental friendliness and reproducible feature, while meeting Future Society energy demand, also meet the theory of the sustainable Scientific Outlook on Development and recycling economy, therefore develop and use bioenergy to become the important component part of developed country of world today energy strategy.
But, account for more than 60% of total cost at the process Raw of preparation biological boat coal/biofuel, therefore how to obtain scale supply, cheapness, the oil resource that can be used as power applications are biological boat coal/Biodieselization core that must solve and key issue.Suitable raw material production biofuel is selected according to national conditions one after another in current countries in the world, as the U.S. mainly utilizes high-yield transgenic soybean to prepare biofuel; European Countries implant mass rape, utilizes rapeseed oil production biofuel; Southeast Asian countries utilizes plam oil as production of biodiesel raw material; Japan then mainly adopts waste cooking oil to carry out production biofuel etc.And China is vast in territory, available Vegetable oil lipoprotein is a lot, and wherein the herbaceous plant such as vegetable seed, soybean is current artificial growth class farm crop the most widely.But because China is populous, herbaceous plant grease yield still can not meet the market requirement of edible oil, therefore food oils can not be used for scale operation biofuel.And the traditional oil tree fruits such as Jatropha curcus, Wood of Shinyleaf Yellowhorn, wilson dogwood, Chinese pistache have that oleaginousness is high, wide accommodation, the drought-resistant feature such as barren, can in mountain region, plateau, knob even sand ground plantation, not only meet the development principle that China's biomass energy " does not strive grain with people; do not strive ground with grain ", and rural economic development of improving the ecological environment, transform agricultural production, promote, all tools such as to increase farmers' income are of great significance.Simultaneously, China is as an edible oil consumption big country, the waste grease total amount that the approach such as annual foodstuff production, changing food waste produce reaches more than 6,500,000 tons, through process further, the raw material that can become biological boat coal/biofuel uses, so not only significantly can reduce the production cost of biofuel, and the rational utilization to waste grease, prevent waste grease from again entering food chain and promote that the development of biological boat coal/biofuel is all very favourable.
The oleaginousness of woody oleiferous plants seed is higher, and the grease usually adopting mechanical expression or mode solvent extraction to produce is referred to as crude oil.In animals and plants crude oil, more than 95% is triglyceride level, in addition also have the impurity such as a certain amount of free fatty acids, phosphatide, metal, pigment, sulfide, nitride, these impurity have very large impact to the technique of hydrogenation method preparation biological boat coal/biofuel, catalyzer and quality product.Therefore, no matter which kind of oil resource, all has to pass through refining and can meet biological boat coal/biodiesel processes to the requirement of raw material.
Chemical refining is a kind of traditional vegetable oil fine smelting method, generally comprises to come unstuck, neutralize the operation such as (alkali refining), decolouring, deodorization.Come unstuck and mainly remove the impurity such as phosphatide, protein and sugar fat; Neutralization is by the free fatty acids in alkali and in grease; Decolouring is the unsaponifiables such as the pigment utilized in the absorb oils such as carclazyte; Deodorization is that the method for wet distillation is except the trace impurity in degrease.The method of the chemical refinings such as use is come unstuck as disclosed in patent CN1147009A, CN1749380A, CN104021A, CN1147011A, neutralization carrys out the grease of production different standards.The operation of chemical refining is many, operational path long, energy consumption is also large.Neutralize (alkali refining) not only can cause free fatty acids to lose simultaneously, and the Chinese honey locust produced can carry the triglyceride level of 20 ~ 50% secretly, causes refining losses rate to increase.In addition due to needs laundry soap compound, therefore also can produce waste water, the COD value of these waste water is higher, difficult treatment.Although equipment and process is updated in recent years, but chemical refining principle never changes over nearly 70 years, and adopting chemical refining technique to carry out refining animal-plant oil, the feedstock specifications that the refining oil obtained can not reach hydrogenation method preparation biological boat coal/biofuel completely requires (phosphorus content is less than 3ug/g, metal is less than 5ug/g, unsaponifiables be less than 0.5% etc.).Therefore, a kind of raw oil refining technique can be adopted, while removing the impurity such as phosphatide, metal, pigment, the free fatty acids do not lost in grease, and meet the feedstock specifications requirement of hydrogenation method preparation biological boat coal/biofuel, become the task of top priority of oil and fat refining industry.
Summary of the invention
The object of the present invention is to provide a kind of preparation method being applicable to the non-edible crude oil refining oil of hydrogenation method preparation biological boat coal/biodiesel raw material requirement, utilize the method can remove the impurity such as phosphatide, metal, pigment in different quality crude oil efficiently and keep the acid number in grease constant.Little, the non-wastewater discharge of refining process grease loss simultaneously.
Preparation method's process of non-edible crude oil refining oil of the present invention is as follows.
(1) filtered by the crude oil squeezed or extract, removing solid particle polluter wherein, is then heated to 40 ~ 80 DEG C;
(2) under the agitation condition of 100 ~ 1000 revs/min, add conversion-complexing agent that quality is crude oil 1 ~ 3% respectively, constant temperature stirs 50 ~ 90min.Reaction terminates rear employing centrifugation, obtains degummed oil and You Jiao;
(3) degummed oil dewaters under vacuum tightness 0.07 ~ 0.09MPa, temperature 95 ~ 105 DEG C, time 15 ~ 25min condition, removes the minor amount of water in grease;
(4) under the condition stirred, the grease after dehydration is heated to 90 ~ 110 DEG C, then adds the sorbent material of 1 ~ 4%, constant temperature stirs 10 ~ 30min, filters and obtains refining oil.
The crude oil used in above-mentioned refining process is Jatropha curcus, Chinese pistache, Wood of Shinyleaf Yellowhorn, wilson dogwood, Aleurites montana, sea-buckthorn, oil tea, tung oil tree, Chinese tallow tree, sewer oil, butter, sheep oil, one or more in lard.
Conversion-complexing agent is one or more in hydrochloric acid, carbonic acid, phosphoric acid, sulfuric acid, citric acid, formic acid, oxalic acid, tartrate, maleic acid, diacetyl oxide, water.
Sorbent material is one or more in silica gel, gac, diatomite, silicon-dioxide, acidic white earth, ion exchange resin, carbon fiber, carbonaceous molecular sieve, active calcium oxide.
The present invention is applicable to the crude oil of different quality, different acid number, and keeps the acid number in grease constant in the course of processing, thus decreases loss, improves refining yield; Eliminate washing and deodorising process simultaneously, because this simplify refinery practice flow process, reducing energy consumption and non-wastewater discharge, greatly save production cost.Refining efficiency of the present invention and stability high, can large-scale operate continuously be carried out.
The feedstock specifications that gained refining oil quality reaches hydrogenation method preparation biological boat coal/biofuel completely requires (phosphorus is less than 3ug/g, metal is less than 5ug/g, unsaponifiables be less than 0.5% etc.).
Embodiment
Embodiment 1
100g Jatropha curcus crude oil (phosphorus content 231ug/g, metal 165ug/g, unsaponifiables 0.6%, acid number 4.8mgKOH/g) is heated to 60 DEG C, under 500 revs/min of agitation conditions, add the citric acid solution 2.6g that concentration is 0.5%, constant temperature obtains degummed oil through centrifugation after stirring 60min.Degummed oil through vacuum hydro-extraction process, then under 90 DEG C, 200 revs/min agitation conditions, adds 3.0g silica gel under vacuum tightness 0.08MPa, temperature 90 DEG C, time 20min condition, filters and obtain refining oil after reaction 30min.The phosphorus content 1.8ug/g of product, metal 4.1ug/g, unsaponifiables 0.4%, acid number 4.8mgKOH/g, meet the feedstock specifications requirement of hydrogenation method preparation biological boat coal/biofuel.
Embodiment 2
100g Jatropha curcus crude oil and sewer oil are mixed (phosphorus content 123ug/g, metal 144ug/g, unsaponifiables 0.58%, acid number 6.9mgKOH/g) grease by 1:1 and is heated to 60 DEG C, under 500 revs/min of agitation conditions, add the citric acid solution 3.0g that concentration is 0.5%, constant temperature obtains degummed oil through centrifugation after stirring 60min.Degummed oil through vacuum hydro-extraction process, then under 90 DEG C, 200 revs/min agitation conditions, adds 3.5g silica gel under vacuum tightness 0.08MPa, temperature 90 DEG C, time 20min condition, filters and obtain refining oil after reaction 30min.The phosphorus content 1.3ug/g of product, metal 3.5ug/g, unsaponifiables 0.44%, acid number 6.9mgKOH/g, meet the feedstock specifications requirement of hydrogenation method preparation biological boat coal/biofuel.
Embodiment 3
100g Jatropha curcus crude oil and sewer oil are mixed (phosphorus content 123ug/g, metal 144ug/g, unsaponifiables 0.58%, acid number 6.9mgKOH/g) grease by 1:1 and is heated to 60 DEG C, under 500 revs/min of agitation conditions, add concentration is 0.5%, ratio is 1:1 citric acid and solution of acetic anhydride 2.0g, constant temperature obtains degummed oil through centrifugation after stirring 60min.Degummed oil through vacuum hydro-extraction process, then under 90 DEG C, 200 revs/min agitation conditions, adds gac and the silica gel of 4.0g under vacuum tightness 0.08MPa, temperature 90 DEG C, time 20min condition, filters and obtain refining oil after reaction 30min.The phosphorus content 0.9ug/g of product, metal 2.9ug/g, unsaponifiables 0.35%, acid number 6.9mgKOH/g, meet the feedstock specifications requirement of hydrogenation method preparation biological boat coal/biofuel.
Embodiment 4
By 100g Chinese pistache crude oil (phosphorus content 183ug/g, metal 101ug/g, unsaponifiables 0.8%, acid number 8.1mgKOH/g) heat to 80 DEG C, under 600 revs/min of agitation conditions, add the citric acid solution 1.5g that concentration is 0.4%, constant temperature obtains degummed oil through centrifugation after stirring 60min.Degummed oil through vacuum hydro-extraction process, then under 105 DEG C, 300 revs/min agitation conditions, adds 3.0g gac under vacuum tightness 0.09MPa, temperature 100 DEG C, time 20min condition, filters and obtain refining oil after reaction 30min.The phosphorus content 0.8ug/g of product, metal 2.9ug/g, unsaponifiables 0.45%, acid number 8.1mgKOH/g, meet the feedstock specifications requirement of hydrogenation method preparation biological boat coal/biofuel.
Embodiment 5
By 100g Chinese pistache crude oil (phosphorus content 183ug/g, metal 101ug/g, unsaponifiables 0.8%, acid number 8.1mgKOH/g) heat to 80 DEG C, under 700 revs/min of agitation conditions, add the citric acid solution 2.0g that concentration is 0.4%, constant temperature obtains degummed oil through centrifugation after stirring 60min.Degummed oil through vacuum hydro-extraction process, then under 105 DEG C, 300 revs/min agitation conditions, adds 4.0g gac under vacuum tightness 0.09MPa, temperature 100 DEG C, time 20min condition, filters and obtain refining oil after reaction 30min.The phosphorus content 1.0ug/g of product, metal 3.3ug/g, unsaponifiables 0.44%, acid number 8.1mgKOH/g, meet the feedstock specifications requirement of hydrogenation method preparation biological boat coal/biofuel.
Embodiment 6
100g Chinese pistache crude oil and oil tea are pressed 1:1 and mix (phosphorus content 130ug/g, metal 96ug/g, unsaponifiables 0.66%, acid number 6.8mgKOH/g) grease heat to 80 DEG C, under 800 revs/min of agitation conditions, add the oxalic acid solution 1.8g that concentration is 0.4%, constant temperature obtains degummed oil through centrifugation after stirring 60min.Degummed oil through vacuum hydro-extraction process, then under 105 DEG C, 300 revs/min agitation conditions, adds 4g gac under vacuum tightness 0.09MPa, temperature 100 DEG C, time 20min condition, filters and obtain refining oil after reaction 30min.The phosphorus content 0.5ug/g of product, metal 2.2ug/g, unsaponifiables 0.48%, meet the feedstock specifications requirement of hydrogenation method preparation biological boat coal/biofuel.
Embodiment 7
100g wilson dogwood crude oil (phosphorus content 128ug/g, metal 102ug/g, unsaponifiables 0.55%, acid number 5.7mgKOH/g) is heated to 70 DEG C, under 500 revs/min of agitation conditions, add the citric acid solution 3g that concentration is 0.5%, constant temperature obtains degummed oil through centrifugation after stirring 60min.Degummed oil through vacuum hydro-extraction process, then under 90 DEG C, 200 revs/min agitation conditions, adds 2.5g ion exchange resin under vacuum tightness 0.08MPa, temperature 90 DEG C, time 20min condition, filters and obtain refining oil after reaction 30min.The phosphorus content 2.0ug/g of product, metal 3.8ug/g, unsaponifiables 0.43%, meet the feedstock specifications requirement of hydrogenation method preparation biological boat coal/biofuel.
Embodiment 8
100g wilson dogwood crude oil, butter and sewer oil are mixed (phosphorus content 142ug/g, metal 119ug/g, unsaponifiables 0.59%, acid number 9.6mgKOH/g) grease by 1:1:1 and is heated to 70 DEG C, under 800 revs/min of agitation conditions, adding concentration is the citric acid of 0.5% and the solution 2.4g of diacetyl oxide, and constant temperature obtains degummed oil through centrifugation after stirring 60min.Degummed oil through vacuum hydro-extraction process, then under 90 DEG C, 200 revs/min agitation conditions, adds 4.0g diatomite under vacuum tightness 0.09MPa, temperature 90 DEG C, time 20min condition, filters and obtain refining oil after reaction 30min.The phosphorus content 1.7ug/g of product, metal 3.3ug/g, unsaponifiables 0.41%, acid number 10.5mgKOH/g, meet the feedstock specifications requirement of hydrogenation method preparation biological boat coal/biofuel.
Embodiment 9
100g wilson dogwood crude oil, Chinese tallow tree and sewer oil are mixed (phosphorus content 142ug/g, metal 119ug/g, unsaponifiables 0.59%, acid number 9.6mgKOH/g) grease by 1:1:1 and is heated to 70 DEG C, under 800 revs/min of agitation conditions, adding concentration is the citric acid of 0.5% and the solution 2.0g of diacetyl oxide, and constant temperature obtains degummed oil through centrifugation after stirring 60min.Degummed oil through vacuum hydro-extraction process, then under 105 DEG C, 300 revs/min agitation conditions, adds 3.5g diatomite under vacuum tightness 0.09MPa, temperature 90 DEG C, time 20min condition, filters and obtain refining oil after reaction 30min.The phosphorus content 0.9ug/g of product, metal 2.8ug/g, unsaponifiables 0.37%, meet the feedstock specifications requirement of hydrogenation method preparation biological boat coal/biofuel.
Embodiment 10
100g Wood of Shinyleaf Yellowhorn crude oil (phosphorus content 155ug/g, metal 120ug/g, unsaponifiables 0.51%, acid number 6.6mgKOH/g) is heated to 75 DEG C, under 800 revs/min of agitation conditions, add the oxalic acid solution 3g that concentration is 0.3%, constant temperature obtains degummed oil through centrifugation after stirring 60min.Degummed oil through vacuum hydro-extraction process, then under 105 DEG C, 400 revs/min agitation conditions, adds 3.5g silicon-dioxide and gac under vacuum tightness 0.09MPa, temperature 100 DEG C, time 20min condition, filters and obtain refining oil after reaction 30min.The phosphorus content 2.5ug/g of product, metal 4.1ug/g, unsaponifiables 0.46%, acid number 6.6mgKOH/g, meet the feedstock specifications requirement of hydrogenation method preparation biological boat coal/biofuel.
Embodiment 11
100g Wood of Shinyleaf Yellowhorn crude oil and oil tea are heated to 75 DEG C by the grease of 1:1 mixing (phosphorus content 148ug/g, metal 112ug/g, unsaponifiables 0.50%, acid number 6.4mgKOH/g), under 800 revs/min of agitation conditions, add the oxalic acid solution 3g that concentration is 0.3%, constant temperature obtains degummed oil through centrifugation after stirring 60min.Degummed oil through vacuum hydro-extraction process, then under 105 DEG C, 400 revs/min agitation conditions, adds 3.5g silicon-dioxide and gac under vacuum tightness 0.09MPa, temperature 100 DEG C, time 20min condition, filters and obtain refining oil after reaction 30min.The phosphorus content 1.9ug/g of product, metal 3.9ug/g, unsaponifiables 0.42%, acid number 6.4mgKOH/g, meet the feedstock specifications requirement of hydrogenation method preparation biological boat coal/biofuel.
Embodiment 12
100g Wood of Shinyleaf Yellowhorn crude oil, oil tea, sewer oil and lard are heated to 75 DEG C by the grease of 1:1:1:1 mixing (phosphorus content 171ug/g, metal 136ug/g, unsaponifiables 0.55%, acid number 7.8mgKOH/g), under 800 revs/min of agitation conditions, add the oxalic acid solution 3g that concentration is 0.3%, constant temperature obtains degummed oil through centrifugation after stirring 60min.Degummed oil through vacuum hydro-extraction process, then under 105 DEG C, 400 revs/min agitation conditions, adds 3.0g silicon-dioxide and gac under vacuum tightness 0.09MPa, temperature 100 DEG C, time 20min condition, filters and obtain refining oil after reaction 30min.The phosphorus content 1.5ug/g of product, metal 3.1ug/g, unsaponifiables 0.39%, acid number 7.8mgKOH/g, meet the feedstock specifications requirement of hydrogenation method preparation biological boat coal/biofuel.
Claims (3)
1. a preparation method for non-edible animals and plants crude oil refining oil, is characterized in that:
(1) filtered by the crude oil squeezed or extract, removing solid particle polluter wherein, is then heated to 40 ~ 80 DEG C;
(2) under the agitation condition of 100 ~ 1000 revs/min, add conversion-complexing agent that quality is crude oil 1 ~ 3%, constant temperature stirs 50 ~ 90min, and reaction terminates rear employing centrifugation, obtains degummed oil and You Jiao;
(3) degummed oil dewaters under vacuum tightness 0.07 ~ 0.09MPa, temperature 95 ~ 105 DEG C, time 15 ~ 25min condition, removes the minor amount of water in grease;
(4) under the condition stirred, the grease after dehydration is heated to 90 ~ 110 DEG C, then adds the sorbent material of 1 ~ 4%, constant temperature stirs 10 ~ 30min, filters and obtains refining oil;
Described conversion-complexing agent is one or more in citric acid, oxalic acid, diacetyl oxide;
Described sorbent material to be sorbent material be in silica gel, gac, diatomite, ion exchange resin one or more.
2. a non-edible animals and plants crude oil refining oil, it is characterized in that: the refining oil of the preparation method of non-edible animals and plants crude oil refining oil according to claim 1, phosphorus content < 3ug/g, metal < 5ug/g, unsaponifiables < 0.5%.
3. according to an application for non-edible animals and plants crude oil refining oil according to claim 2, it is characterized in that: non-edible animals and plants crude oil refining oil is as the raw material of hydrogenation method preparation biological boat coal/biofuel.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104073363A (en) * | 2014-06-30 | 2014-10-01 | 李安民 | Degumming and impurity removing process and equipment for waste oil |
| CN104531350B (en) * | 2014-12-05 | 2017-10-27 | 昆明理工大学 | A kind of method for purifying biodiesel |
| CN104611123A (en) * | 2015-02-06 | 2015-05-13 | 长沙市越大油脂有限责任公司 | Extraction process method of animal grease |
| CN105238557A (en) * | 2015-10-26 | 2016-01-13 | 全椒县尹氏油脂有限公司 | Antioxidative refined lard oil |
| CN106281669A (en) * | 2015-11-04 | 2017-01-04 | 云南师范大学 | A kind of preparation method of vegetable oil degumming zeolite |
| CN113528244A (en) * | 2021-06-17 | 2021-10-22 | 罗静 | Method for removing impurities from plant essential oil for cosmetics |
| CN114933930B (en) * | 2022-05-16 | 2024-03-15 | 广汉市迈德乐食品有限公司 | Butter hardness improving method based on compound gel factor |
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