CN101880596A - A method for low temperature preparation of oil - Google Patents
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Abstract
本发明涉及从油料提取油脂的方法。一种油脂低温制取的方法,其特征在于它包括如下步骤:1)清理:除去油料杂质;2)调质:调节油料的温度和水分,调质后的油料温度为5~65℃,油料的质量含水量调节到4~16%;3)低温压榨:将调质后的油料进行压榨,油料的入榨温度为-10~65℃,入榨油料的质量含水量为4~16%,获得毛油;4)脱胶:将毛油温度保持在5~65℃,加入脱胶固体吸附剂,脱胶固体吸附剂的添加量为毛油质量的0.1~5%,脱胶时间为0.1~2h;5)脱酸:将脱胶后的毛油温度保持在5~65℃,加入脱酸固体吸附剂,脱酸固体吸附剂的添加量为脱胶后毛油质量的0.1~2%,脱酸时间为0.1~3h,得到油脂。本发明适用于工业化生产。
The invention relates to a method for extracting fat from oil plants. A method for producing oil at low temperature, which is characterized in that it comprises the following steps: 1) cleaning: removing oil impurities; 2) tempering: adjusting the temperature and moisture of the oil, the temperature of the oil after conditioning is 5-65°C, and the oil is 3) Low-temperature pressing: press the conditioned oil plant, the temperature of the oil plant is -10-65°C, and the mass water content of the oil plant is 4-16%. Obtain crude oil; 4) degumming: keep the temperature of crude oil at 5-65°C, add degumming solid adsorbent, the amount of degumming solid adsorbent added is 0.1-5% of the mass of crude oil, and the degumming time is 0.1-2h; 5 ) Deacidification: Keep the temperature of the degummed crude oil at 5-65°C, add a deacidification solid adsorbent, the amount of the deacidification solid adsorbent is 0.1-2% of the mass of the degummed crude oil, and the deacidification time is 0.1 ~3h, to get oil. The invention is suitable for industrialized production.
Description
技术领域technical field
本发明涉及从油料提取油脂的方法,具体是一种油脂低温制取的方法,属于油脂加工技术领域。The invention relates to a method for extracting oil from oil plants, in particular to a method for preparing oil at low temperature, and belongs to the technical field of oil processing.
背景技术Background technique
目前油脂制取方法较多,应用最广的是压榨法和溶剂浸出法。现有主要的压榨工艺是:清理、轧坯、蒸炒、预榨(压榨),一般蒸炒和压榨温度在100℃以上,其缺点是能量消耗大,毛油磷脂含量高、色泽深,精炼损耗大,同时饼粕蛋白变性程度高,有效氨基酸损失大,饼粕色泽深。溶剂浸出法是利用能溶解油脂的有机溶剂,通过湿润、渗透、分子扩散的作用将油脂萃取出来,但是浸出法存在溶剂残留问题,这些溶剂对人体健康有一定的危害。水代法是将热水加入经过预处理的油籽原料中,利用油水不相溶和水与蛋白亲和力大的原理,用热水把油脂从原料中代替出来;该方法的优点是安全、环保、能耗少、工艺简单,而且油脂品质好,但是适用性窄,一般用于芝麻制油。水酶法是利用酶制剂降解植物油籽细胞壁和脂类复合体,有利于提高油脂的出油率,同时处理条件温和,能同时得到优质的油脂和饼粕蛋白,该工艺简单且能耗低,但是目前酶制剂价格较高,该工艺未形成大规模生产。超临界流体萃取法是利用气体在高压低温下形成超临界流体萃取油脂,此工艺提取的油脂产品富含活性物质且品质好,无有机溶剂残留并且环保,但是该工艺设备要求高,生产成本偏高。超声波辅助萃取法是将超声波技术应用于溶剂浸提法中,提高提油效率和产品品质,但是目前工艺设备造价高,该技术还处于探索阶段。微波辅助萃取油脂技术是在溶剂浸提的基础上,利用微波来提高油脂的提取效率,可以缩短提取时间,降低能耗,减少有机溶剂用量,但是目前该技术并未成熟。At present, there are many methods for oil production, and the most widely used methods are pressing method and solvent extraction method. The existing main pressing processes are: cleaning, billet rolling, steaming and frying, and pre-pressing (pressing). Generally, the temperature of steaming, frying and pressing is above 100°C. The loss is large, and at the same time, the degree of protein denaturation of the cake is high, the loss of effective amino acids is large, and the color of the cake is deep. The solvent leaching method uses an organic solvent that can dissolve oil to extract the oil through the effects of wetting, penetration, and molecular diffusion. However, there is a problem of solvent residue in the leaching method, and these solvents are harmful to human health. The water substitution method is to add hot water to the pretreated oilseed raw material, and use the principle of oil-water immiscibility and high affinity between water and protein to replace the oil from the raw material with hot water; the advantages of this method are safety and environmental protection , less energy consumption, simple process, and good oil quality, but narrow applicability, generally used for sesame oil. The aqueous enzymatic method uses enzyme preparations to degrade the cell walls and lipid complexes of vegetable oilseeds, which is conducive to improving the oil yield of oils. At the same time, the treatment conditions are mild, and high-quality oils and cake proteins can be obtained at the same time. The process is simple and low energy consumption. However, the price of enzyme preparations is relatively high at present, and this process has not formed a large-scale production. Supercritical fluid extraction method is to use gas to form supercritical fluid under high pressure and low temperature to extract oil. The oil product extracted by this process is rich in active substances and has good quality, no organic solvent residue and is environmentally friendly. However, this process requires high equipment and high production cost. high. Ultrasonic-assisted extraction is the application of ultrasonic technology to solvent extraction to improve oil extraction efficiency and product quality. However, the cost of process equipment is currently high, and this technology is still in the exploratory stage. Microwave-assisted oil extraction technology is based on solvent extraction, using microwave to improve the extraction efficiency of oil, which can shorten the extraction time, reduce energy consumption, and reduce the amount of organic solvents, but the technology is not yet mature.
通过上述工艺所获得的油称为毛油,通常毛油需要经过精炼后获得最终产品。目前的油脂精炼过程包括脱胶、脱酸、脱色、脱臭等工序。传统脱胶工艺主要包括水化脱胶和酸法脱胶。水化脱胶只能除去水合性磷脂,而非水合性磷脂却很难脱除。酸法脱胶一般先将毛油加热到70℃以上,然后添加磷酸或柠檬酸等溶液磷脂。酶法脱胶工艺可免去水洗工序,具有精炼率高、脱胶彻底、油脚含油量低、生产成本低等优点,但是成本还是偏高,未能大规模应用。膜脱胶的主要优点有操作条件温和、温度低,工艺简单,减少精炼废水,应用局限主要有膜通量、长期稳定性、膜的清洗再利用等问题。脱酸主要有化学脱酸、物理脱酸和混合油脱酸。化学脱酸特点是快速、高效,适用于各种低酸值油脂,工艺设备技术成熟,缺点是中性油脂损耗较大,尤其不适用于高酸值毛油。物理脱酸适用于高酸值油脂,操作简单,能耗少,油脂损失率可以降到1.05~1.2%,缺点是对毛油预处理要求高而生产成本相对较高,不适合胶质含量高的油脂,同时高温下易产生反式脂肪酸。混合油脱酸优点在于使用的碱溶液浓度低,离心效率高,中性油脂损失低,产品色泽好,但工艺过程复杂,溶剂消耗大,设备投资大。目前国内外出现了一些新的油脂脱酸技术,如生物脱酸、化学再酯化脱酸、溶剂萃取脱酸、超临界萃取脱酸、膜分离技术脱酸、分子蒸馏脱酸等,但这些尚处于研究阶段,未大规模应用。The oil obtained through the above process is called crude oil, and usually the crude oil needs to be refined to obtain the final product. The current oil refining process includes degumming, deacidification, decolorization, deodorization and other processes. The traditional degumming process mainly includes hydration degumming and acid degumming. Hydration degumming can only remove hydratable phospholipids, but non-hydratable phospholipids are difficult to remove. For acid degumming, the crude oil is generally heated above 70°C, and then phosphoric acid or citric acid and other solution phospholipids are added. The enzymatic degumming process can eliminate the washing process, and has the advantages of high refining rate, thorough degumming, low oil content in oil bottoms, and low production costs. However, the cost is still high and cannot be applied on a large scale. The main advantages of membrane degumming are mild operating conditions, low temperature, simple process, and reduced refining wastewater. The application limitations mainly include membrane flux, long-term stability, and membrane cleaning and reuse. Deacidification mainly includes chemical deacidification, physical deacidification and mixed oil deacidification. The characteristics of chemical deacidification are fast and efficient, and it is suitable for various low acid value oils. The process equipment is mature, but the disadvantage is that the loss of neutral oil is large, especially not suitable for high acid value crude oil. Physical deacidification is suitable for oil with high acid value, simple operation, less energy consumption, and the loss rate of oil can be reduced to 1.05-1.2%. The disadvantage is that it requires high pretreatment of crude oil and the production cost is relatively high. It is not suitable for high colloid content. At the same time, it is easy to produce trans fatty acids at high temperature. The advantages of deacidification of mixed oil are the low concentration of alkali solution used, high centrifugation efficiency, low loss of neutral oil, and good color of the product, but the process is complicated, the solvent consumption is large, and the investment in equipment is large. At present, some new oil deacidification technologies have appeared at home and abroad, such as biological deacidification, chemical re-esterification deacidification, solvent extraction deacidification, supercritical extraction deacidification, membrane separation technology deacidification, molecular distillation deacidification, etc., but these It is still in the research stage and has not been applied on a large scale.
CN1840623A公开了一种油料的低温制油及油料蛋白制取方法。它采用低温榨油设备在入榨温度为20~70℃的条件下对油料进行压榨,获得低温压榨毛油和低温压榨饼;毛油经沉淀、精滤后得低温压榨天然油;低温压榨饼使用粉碎设备直接进行超微粉碎加工,获得半脱脂蛋白粉,或采用乙醇等溶液浸出制备浓缩蛋白粉。该技术主要是针对带皮(壳)油料为原料,目的是获得低温压榨毛油和低温压榨饼,然后制取油料蛋白,未涉及到低温毛油的精制工艺。CN1840623A discloses a method for producing oil from oil at low temperature and protein from oil. It uses low-temperature oil pressing equipment to press the oil under the condition of the input temperature of 20-70°C to obtain low-temperature pressed crude oil and low-temperature pressed cake; the crude oil is precipitated and finely filtered to obtain low-temperature pressed natural oil; low-temperature pressed cake Use pulverization equipment to directly carry out superfine pulverization processing to obtain semi-skimmed protein powder, or use ethanol and other solutions to leaching to prepare concentrated protein powder. This technology is mainly aimed at the oil with skin (shell) as raw material, the purpose is to obtain low-temperature pressed crude oil and low-temperature pressed cake, and then produce oil protein, and does not involve the refining process of low-temperature crude oil.
CN1740296A公开了一种低温半精炼压榨大豆油的工艺方法。以大豆为原料,通过精选、破碎、壳仁分离、压坯、蒸炒、压榨、低温水化、渣油分离、干燥、精滤等步骤获得大豆油,其中蒸炒的温度为115-125℃,时间为60min,水化脱胶的温度是50-60℃,水添加量为4-6%。该技术主要针对大豆原料,采用高温蒸炒压榨,所获得的毛油磷脂含量较高,而且水化脱胶只能除去水合性磷脂。CN1740296A discloses a process for semi-refining and pressing soybean oil at low temperature. Using soybeans as raw materials, soybean oil is obtained through the steps of selection, crushing, separation of shell and kernel, pressing, steaming, pressing, low-temperature hydration, separation of residue oil, drying, and fine filtration. The temperature of steaming and frying is 115-125 °C, the time is 60 minutes, the temperature of hydration degumming is 50-60 °C, and the amount of water added is 4-6%. This technology is mainly aimed at soybean raw materials. It uses high-temperature steaming, frying and pressing, and the obtained crude oil phospholipids have a high content, and hydration degumming can only remove hydratable phospholipids.
CN1434849A公开了一种精炼动植物油的方法。该技术处理动植物油的方法是采用吸附性二氧化硅,吸附性二氧化硅吸附了其中的非甘油三酯化合物以及很少量的甘油三酯,通过分离二氧化硅以制备精炼油,而分离的二氧化硅可以用作动物饲料添加剂。该技术主要针对油脂精炼方法,在常温下,通过吸附性二氧化硅去除非甘油三酯化合物,未涉及到油脂制取工艺。CN1434849A discloses a method for refining animal and vegetable oils. The method of this technology to treat animal and vegetable oils is to use adsorbent silica, which absorbs non-triglyceride compounds and a small amount of triglyceride, and separates silica to prepare refined oil. Silica can be used as an animal feed additive. This technology is mainly aimed at the oil refining method. At room temperature, non-triglyceride compounds are removed through adsorbed silica, and no oil production process is involved.
CN101485365A公开了一种油脂的精制方法。采用超滤膜在25~55℃下脱胶处理10~30h,再经纳滤膜25~55℃下进行脱酸处理40~70h,最后于220~250℃、50~200Pa下脱臭即得精制油脂。该技术是一种物理精炼方法,其中脱胶和脱酸在较低温度下进行,但是处理时间太长,同时清理膜使用到脂肪酶溶液,成本高。CN101485365A discloses a method for refining oil. Use ultrafiltration membrane to degumming treatment at 25~55℃ for 10~30h, then conduct deacidification treatment at 25~55℃ for 40~70h through nanofiltration membrane, and finally deodorize at 220~250℃ and 50~200Pa to obtain refined oil . This technology is a physical refining method, in which degumming and deacidification are carried out at a lower temperature, but the treatment time is too long, and lipase solution is used to clean the membrane at the same time, and the cost is high.
从上述油料、油脂制取以及油脂精炼技术来看,各有一定的弊端,同时未涉及到完整的油脂低温制取与精制的方法。From the perspective of the above-mentioned oil plants, oil production and oil refining technologies, each has certain disadvantages, and does not involve a complete low-temperature oil production and refining method.
发明内容Contents of the invention
本发明的目的是提供一种适用于工业化生产的油脂低温制取的方法。The purpose of the present invention is to provide a method for producing oil at low temperature suitable for industrial production.
为了实现上述目的,本发明采用以下技术方案:一种油脂低温制取的方法,其特征在于它包括如下步骤:In order to achieve the above object, the present invention adopts the following technical solutions: a method for producing oil at low temperature, characterized in that it comprises the following steps:
1)清理:除去油料杂质;1) Cleaning: remove oil impurities;
2)调质:调节油料的温度和水分,调质后的油料温度为5~65℃,油料的质量含水量调节到4~16%;2) Quenching and tempering: adjust the temperature and moisture of the oil, the temperature of the oil after conditioning is 5-65°C, and the mass water content of the oil is adjusted to 4-16%;
3)低温压榨:将调质后的油料进行压榨,油料的入榨温度为-10~65℃,入榨油料的质量含水量为4~16%,获得毛油;3) Low-temperature pressing: press the conditioned oil, the temperature of the oil is -10-65°C, and the water content of the oil is 4-16%, to obtain crude oil;
4)脱胶:将毛油温度保持在5~65℃,加入脱胶固体吸附剂,脱胶固体吸附剂的添加量为毛油质量的0.1~5%,脱胶时间为0.1~2h;4) Degumming: keep the crude oil temperature at 5-65°C, add degumming solid adsorbent, the amount of degumming solid adsorbent added is 0.1-5% of the crude oil mass, and the degumming time is 0.1-2h;
5)脱酸:将脱胶后的毛油温度保持在5~65℃,加入脱酸固体吸附剂,脱酸固体吸附剂的添加量为脱胶后毛油质量的0.1~2%,脱酸时间为0.1~3h,得到油脂(天然原生态油脂)。5) Deacidification: keep the temperature of the degummed crude oil at 5-65°C, add a deacidification solid adsorbent, the amount of the deacidification solid adsorbent is 0.1-2% of the mass of the degummed crude oil, and the deacidification time is 0.1 to 3 hours to obtain oil (natural original ecological oil).
步骤1)所述的油料作物可以是油菜籽、大豆、油茶籽、茶叶籽、花生、胡麻、芝麻、葵花籽、棉籽、核桃、紫苏、葡萄籽、油橄榄、米糠、玉米胚、蓖麻或乌桕。The oil crops described in step 1) can be rapeseed, soybean, camellia seed, tea seed, peanut, flax, sesame, sunflower seed, cottonseed, walnut, perilla, grape seed, olive, rice bran, corn germ, castor or Chinese tallow tree.
步骤2)调质后的油料脱皮(壳)或不脱皮(壳):油料的脱皮(壳)率为60-99.5wt%[脱壳率=(已脱壳的油料重量/油料总重量)×100%]。Step 2) peeling (shell) or non-peeling (shell) of the oil plant after conditioning: the peeling (shell) rate of the oil plant is 60-99.5wt% [the shelling rate=(the weight of the oil plant that has been shelled/the total weight of the oil plant) × 100%].
所述的低温是指-10~65℃。The low temperature refers to -10-65°C.
所述的脱胶固体吸附剂由①膨润土,②硅酸盐,③二氧化硅,④磷酸或柠檬酸四种原料制备而成,各原料所占质量百分数为:The degummed solid adsorbent is prepared from four raw materials: ① bentonite, ② silicate, ③ silicon dioxide, ④ phosphoric acid or citric acid, and the mass percentages of each raw material are:
膨润土:30-60%,Bentonite: 30-60%,
硅酸盐:20-50%,Silicate: 20-50%,
二氧化硅:10-40%,Silica: 10-40%,
磷酸或柠檬酸:0.1-3%。Phosphoric acid or citric acid: 0.1-3%.
所述的脱胶固体吸附剂的制备方法为:按各原料所占质量百分数为:The preparation method of described degummed solid adsorbent is: according to the mass percentage that each raw material accounts for:
膨润土:30-60%,Bentonite: 30-60%,
硅酸盐:20-50%,Silicate: 20-50%,
二氧化硅:10-40%,Silica: 10-40%,
磷酸或柠檬酸:0.1-3%,Phosphoric acid or citric acid: 0.1-3%,
选取①膨润土,②硅酸盐,③二氧化硅,④磷酸或柠檬酸四种原料,备用;Select ①bentonite, ②silicate, ③silicon dioxide, ④phosphoric acid or citric acid four raw materials, set aside;
将膨润土、硅酸盐、二氧化硅分别进行干燥处理,然后分别粉碎处理,粗细粒度为20目~200目;然后将膨润土、硅酸盐和二氧化硅与磷酸或柠檬酸进行均匀混合,即获得脱胶固体吸附剂。Dry bentonite, silicate, and silicon dioxide separately, and then pulverize them separately, with a particle size of 20 mesh to 200 mesh; then uniformly mix bentonite, silicate, and silicon dioxide with phosphoric acid or citric acid, that is A degummed solid adsorbent is obtained.
所述的脱酸固体吸附剂由碱性化合物和油料作物种籽壳原料制备而成,各原料所占质量百分数为:碱性化合物2-35%,油料作物种籽壳65-98%;所述的油料作物种籽壳为油茶壳、花生壳、葵花籽壳、蓖麻壳、核桃壳中的任意一种或任意二种以上的混合,任意二种以上混合时为任意配比。The deacidification solid adsorbent is prepared from basic compounds and oil crop seed shell raw materials, and the mass percentages of each raw material are: 2-35% of basic compounds and 65-98% of oil crop seed shells; The seed shells of the oil crops mentioned above are any one of camellia oleifera shell, peanut shell, sunflower seed shell, castor bean shell, and walnut shell, or any two or more of them, and any two or more of them are mixed in any ratio.
所述的碱性化合物为氢氧化钾、氢氧化钠、氢氧化钙、碳酸钠、碳酸钾中的任意一种或任意二种以上的混合,任意二种以上混合时为任意配比。The basic compound is any one of potassium hydroxide, sodium hydroxide, calcium hydroxide, sodium carbonate, and potassium carbonate, or a mixture of any two or more of them. When any two or more of them are mixed, the ratio is arbitrary.
所述的脱酸固体吸附剂的制备方法:The preparation method of described deacidification solid adsorbent:
1)原料选取:按各原料所占质量百分数为:碱性化合物2-35%,油料作物种籽壳65-98%,选取碱性化合物和油料作物种籽壳;1) Selection of raw materials: according to the mass percentage of each raw material: 2-35% of the basic compound, 65-98% of the seed shell of the oil crop, the basic compound and the seed shell of the oil crop are selected;
2)活化:将油料作物种籽壳进行清理,然后在60~110℃条件下干燥,再在150~500℃条件下活化,获得活化物;2) Activation: cleaning the seed shells of oil crops, then drying at 60-110°C, and then activating at 150-500°C to obtain activated products;
3)粉碎:将活化物粉碎至20目~100目;3) Pulverization: pulverize the active substance to 20 mesh to 100 mesh;
4)吸附:将碱性化合物配制成浓度为5~45wt%含碱性化合物的水溶液,将粉碎后的活化物置于容器中,加入含碱性化合物的水溶液,在20~80℃下搅拌0.5h~5h;搅拌后过滤,分离出固体物;4) Adsorption: Prepare the basic compound into an aqueous solution containing the basic compound at a concentration of 5-45 wt%, put the pulverized active substance in a container, add the aqueous solution containing the basic compound, and stir at 20-80°C for 0.5h ~5h; Stir and filter to separate the solid;
5)干燥:将固体物进行干燥,得到脱酸固体吸附剂。5) Drying: drying the solid matter to obtain a deacidified solid adsorbent.
所述的活化处理中的干燥时间为1h~3h;活化时间为1h~7h。The drying time in the activation treatment is 1h-3h; the activation time is 1h-7h.
本发明的有益效果是:The beneficial effects of the present invention are:
(1)本发明采用低温(-10~65℃)制取油脂,适用于工业化生产。(1) The present invention uses low temperature (-10 to 65° C.) to prepare oil and fat, which is suitable for industrial production.
(2)本发明采用纯物理压榨制油,带皮(壳)或不带皮(壳)油料原料均适合,入榨油料温度低,水分要求范围宽,压榨获得的毛油色泽浅,保持原料特有风味;(2) The present invention adopts pure physical pressing to make oil, and the oil material with skin (shell) or without skin (shell) is suitable. unique flavor;
本发明制备的油料压榨饼色泽浅,蛋白变性程度低,有效氨基酸损失程度低;同时经过脱皮(壳)处理过的压榨饼的纤维含量降低,适口性提高。The oil press cake prepared by the invention has light color, low degree of protein denaturation and low loss of effective amino acid; at the same time, the fiber content of the pressed cake treated by peeling (shell) is reduced, and the palatability is improved.
(3)本发明的油脂的精制(从毛油至油脂)是采用固体吸附剂进行脱胶和脱酸处理,无溶剂残留,精炼率高,无废水排放,能耗消耗低;精制后的成品油脂仍保持原生态风味,富含微量营养成分。(3) The refining (from crude oil to grease) of the present invention is to adopt solid adsorbent to carry out degumming and deacidification treatment, no solvent residue, high refining rate, no waste water discharge, low energy consumption; refined finished oil It still maintains the original ecological flavor and is rich in micronutrients.
(4)本发明可广泛适用于不同种类的油料。(4) The present invention can be widely applied to different kinds of oil plants.
附图说明Description of drawings
图1是本发明的工艺流程示意图。Fig. 1 is a process flow diagram of the present invention.
具体实施方式Detailed ways
为了更好地理解本发明,下面结合实施例进一步阐明本发明的内容,但本发明的内容不仅仅局限于下面的实施例。In order to better understand the present invention, the content of the present invention is further illustrated below in conjunction with the examples, but the content of the present invention is not limited to the following examples.
实施例1:Example 1:
如图1所示,一种油脂低温制取的方法,它包括如下步骤:As shown in Figure 1, a kind of method for oil and fat low temperature preparation, it comprises the steps:
1)清理:以油菜籽为原料,进行清理除杂;1) cleaning: use rapeseed as raw material to clean and remove impurities;
2)调质:然后将油菜籽的水分干燥至7wt%,油菜籽冷却至50℃;2) conditioning: then drying the moisture of the rapeseed to 7wt%, and cooling the rapeseed to 50°C;
3)低温压榨:采用油菜籽脱壳分离机对调质后的油菜籽进行脱皮分离,测定脱皮率为95%,得到油菜籽仁;收集油菜籽仁,采用螺旋压榨机进行压榨,入榨温度为35℃,入榨油菜籽仁的水分含量为8wt%;得到菜籽毛油;3) Low-temperature pressing: use a rapeseed shelling separator to peel and separate the conditioned rapeseed, measure the peeling rate to 95%, and obtain rapeseed kernels; collect the rapeseed kernels, and use a screw press to squeeze them, and the temperature for pressing is 35 DEG C, the moisture content of the rapeseed kernel that goes into the press is 8wt%; Obtain rapeseed crude oil;
4)脱胶:将菜籽毛油进行离心分离除去沉淀物,测定酸值为1.56mgKOH/g,然后将菜籽毛油的温度保持在30℃,加入菜籽毛油质量0.5%的脱胶固体吸附剂,脱胶时间为0.5h;接着离心分离获得脱胶菜籽油,进行加热试验分析,分析结果是无析出物,黄色值和红色值均不变;4) Degumming: Centrifuge the crude rapeseed oil to remove the sediment, measure the acid value to 1.56mgKOH/g, then keep the temperature of the crude rapeseed oil at 30°C, add 0.5% of the crude rapeseed oil to the degummed solid for adsorption agent, the degumming time is 0.5h; then centrifuged to obtain degummed rapeseed oil, heat test analysis, the analysis result is no precipitate, yellow value and red value are all unchanged;
5)脱酸:将脱胶菜籽油的温度保持在35℃,加入脱胶菜籽油质量1.2%的脱酸固体吸附剂,脱酸时间为0.5h,接着离心分离获得油脂(天然原生态油脂,或称脱酸菜籽油),测定酸值为0.30mgKOH/g,中性油得率为97.6%。5) Deacidification: keep the temperature of the degummed rapeseed oil at 35° C., add a deacidification solid adsorbent with a mass of 1.2% of the degummed rapeseed oil, and deacidify for 0.5 h, then centrifuge to obtain oil (natural original ecological oil, or deacidified rapeseed oil), the measured acid value is 0.30mgKOH/g, and the yield of neutral oil is 97.6%.
所述的脱胶固体吸附剂由①膨润土,②硅酸盐,③二氧化硅,④磷酸四种原料制备而成,各原料所占质量百分数为:膨润土:45%,硅酸盐:35%,二氧化硅:19%,磷酸:1%;The degummed solid adsorbent is prepared from four raw materials: ① bentonite, ② silicate, ③ silicon dioxide, and ④ phosphoric acid. The mass percentages of each raw material are: bentonite: 45%, silicate: 35%, Silica: 19%, phosphoric acid: 1%;
其制备方法为:将膨润土、硅酸盐、二氧化硅分别进行干燥处理,然后分别粉碎处理,粗细粒度为20目~200目;然后将膨润土、硅酸盐和二氧化硅与磷酸进行均匀混合,即获得脱胶固体吸附剂。The preparation method is as follows: dry bentonite, silicate and silicon dioxide respectively, and then pulverize them separately, with a coarse and fine particle size of 20 mesh to 200 mesh; then uniformly mix bentonite, silicate and silicon dioxide with phosphoric acid , to obtain degummed solid adsorbent.
所述的脱酸固体吸附剂由碱性化合物和油料作物种籽壳原料制备而成,各原料所占质量百分数为:碱性化合物20%,油料作物种籽壳80%;所述的油料作物种籽壳为油茶壳;所述的碱性化合物为氢氧化钾;The deacidification solid adsorbent is prepared from basic compounds and oil crop seed shell raw materials, and the mass percentage of each raw material is: 20% of basic compound, 80% of oil crop seed shell; the oil crop The seed shell is camellia oleifera shell; the basic compound is potassium hydroxide;
其制备方法为:Its preparation method is:
1)原料选取:按上述配比选取;1) Raw material selection: select according to the above ratio;
2)活化:将油料作物种籽壳进行清理,然后在90℃条件下干燥,干燥时间为2h;再在300℃条件下活化,活化时间为4h,获得活化物;2) Activation: Clean the seed husks of oil crops, and then dry them at 90°C for 2 hours; then activate them at 300°C for 4 hours to obtain activated products;
3)粉碎:将活化物粉碎至60目;3) Pulverization: pulverize the active substance to 60 mesh;
4)吸附:将碱性化合物配制成浓度为25wt%含碱性化合物的水溶液,将粉碎后的活化物置于容器中,加入含碱性化合物的水溶液,在50℃下搅拌2h;搅拌后过滤,分离出固体物;4) Adsorption: prepare the basic compound into an aqueous solution containing a basic compound at a concentration of 25 wt%, put the pulverized active substance in a container, add the aqueous solution containing a basic compound, and stir at 50° C. for 2 hours; filter after stirring, solids are separated;
5)干燥:将固体物进行干燥,得到脱酸固体吸附剂。5) Drying: drying the solid matter to obtain a deacidified solid adsorbent.
实施例2:Example 2:
如图1所示,一种油脂低温制取的方法,它包括如下步骤:As shown in Figure 1, a kind of method for oil and fat low temperature preparation, it comprises the steps:
1)清理:以大豆为原料,进行清理除杂;1) cleaning: using soybeans as raw materials to clean and remove impurities;
2)调质:然后将大豆的水分干燥至9wt%,冷却大豆至45℃;2) conditioning: then dry the moisture of soybeans to 9wt%, and cool soybeans to 45°C;
3)低温压榨:采用螺旋压榨机直接进行压榨,入榨温度为45℃,大豆的水分含量为9wt%;得到大豆毛油;3) Low-temperature pressing: direct pressing with a screw press, the pressing temperature is 45°C, and the moisture content of soybeans is 9wt%; crude soybean oil is obtained;
4)脱胶:将大豆毛油进行离心分离除去沉淀物,测定酸值为2.05mgKOH/g,然后将大豆毛油的温度保持在40℃,加入大豆毛油质量1.5%的脱胶固体吸附剂,处理时间为0.6h,接着离心分离获得脱胶大豆油,进行加热试验分析,分析结果是无析出物,黄色值和红色值均不变;4) Degumming: Centrifuge the crude soybean oil to remove the sediment, measure the acid value to 2.05mgKOH/g, then keep the temperature of the crude soybean oil at 40°C, add a degumming solid adsorbent with a mass of 1.5% of the crude soybean oil, and process The time is 0.6h, followed by centrifugation to obtain degummed soybean oil, which is analyzed by heating test. The analysis result shows that there is no precipitate, and the yellow value and red value remain unchanged;
5)脱酸:将脱胶大豆油的温度保持在40℃,加入脱胶大豆油质量2%的脱酸固体吸附剂,处理时间为0.8h,接着离心分离获得油脂(天然原生态油脂,或称脱酸大豆油),测定酸值为0.20mgKOH/g,中性油得率为96.9%。5) Deacidification: keep the temperature of the degummed soybean oil at 40°C, add a deacidified solid adsorbent with 2% of the mass of the degummed soybean oil, the treatment time is 0.8h, and then centrifuge to obtain oil (natural original ecological oil, or deacidified oil). sour soybean oil), the measured acid value is 0.20mgKOH/g, and the yield of neutral oil is 96.9%.
所述的脱胶固体吸附剂由①膨润土,②硅酸盐,③二氧化硅,④柠檬酸四种原料制备而成,各原料所占质量百分数为:膨润土:40%,硅酸盐:30%,二氧化硅:28%,柠檬酸:2%;The degummed solid adsorbent is prepared from four raw materials: ① bentonite, ② silicate, ③ silicon dioxide, and ④ citric acid. The mass percentages of each raw material are: bentonite: 40%, silicate: 30% , silicon dioxide: 28%, citric acid: 2%;
其制备方法为:将膨润土、硅酸盐、二氧化硅分别进行干燥处理,然后分别粉碎处理,粗细粒度为150目;然后将膨润土、硅酸盐和二氧化硅与柠檬酸进行均匀混合,即获得脱胶固体吸附剂。The preparation method is as follows: drying bentonite, silicate and silicon dioxide respectively, and then pulverizing them respectively, with a particle size of 150 meshes; then uniformly mixing bentonite, silicate and silicon dioxide with citric acid, namely A degummed solid adsorbent is obtained.
所述的脱酸固体吸附剂由碱性化合物和油料作物种籽壳原料制备而成,各原料所占质量百分数为:碱性化合物25%,油料作物种籽壳75%;所述的油料作物种籽壳为花生壳;所述的碱性化合物为氢氧化钠;The deacidification solid adsorbent is prepared from basic compounds and oil crop seed shell raw materials, and the mass percentage of each raw material is: 25% of basic compound, 75% of oil crop seed shell; the oil crop The seed shell is peanut shell; the basic compound is sodium hydroxide;
其制备方法:Its preparation method:
1)原料选取:按上述配比选取;1) Raw material selection: select according to the above ratio;
2)活化:将油料作物种籽壳进行清理,然后在100℃条件下干燥1h,再在300℃条件下活化5h,获得活化物;2) Activation: Clean the seed shells of oil crops, then dry them at 100°C for 1 hour, and then activate them at 300°C for 5 hours to obtain activated products;
3)粉碎:将活化物粉碎至80目;3) Pulverization: pulverize the active substance to 80 mesh;
4)吸附:将碱性化合物配制成浓度为25wt%含碱性化合物的水溶液,将粉碎后的活化物置于容器中,加入含碱性化合物的水溶液,在60℃下搅拌3h;搅拌后过滤,分离出固体物;4) Adsorption: prepare the basic compound into an aqueous solution containing a basic compound with a concentration of 25 wt%, put the pulverized active substance in a container, add the aqueous solution containing a basic compound, and stir for 3 hours at 60° C.; filter after stirring, solids are separated;
5)干燥:将固体物进行干燥,得到脱酸固体吸附剂。5) Drying: drying the solid matter to obtain a deacidified solid adsorbent.
实施例3:Example 3:
如图1所示,一种油脂低温制取的方法,它包括如下步骤:As shown in Figure 1, a kind of method for oil and fat low temperature preparation, it comprises the steps:
1)清理:以油茶籽为原料,进行清理除杂,1) Cleaning: use camellia oleifera seed as raw material to clean and remove impurities,
2)调质:然后将油茶籽的水分干燥至7.5wt%,冷却油茶籽至35℃;2) conditioning: then drying the moisture of the camellia oleifera seed to 7.5wt%, and cooling the camellia oleifera seed to 35°C;
3)低温压榨:采用油茶籽脱壳分离机对油茶籽进行脱壳分离,测定脱壳率为90%;收集油茶籽仁,采用螺旋压榨机进行压榨,入榨温度为30℃,水分含量为7.5wt%;得到茶籽毛油;3) Low-temperature pressing: the camellia oleifera seed is shelled and separated by a camellia seed shelling separator, and the shelling rate is determined to be 90%; the camellia oleifera seed kernel is collected and pressed by a screw press. The temperature for pressing is 30° C., and the moisture content is 7.5wt%; Obtain tea seed crude oil;
4)脱胶:将茶籽毛油进行离心分离除去沉淀物,测定酸值为1.80mgKOH/g,然后将油茶籽毛油的温度保持在30℃,加入油茶籽毛油质量1%的脱胶固体吸附剂,处理时间为0.3h,接着离心分离获得脱胶茶籽油,进行加热试验分析,分析结果是无析出物,黄色值和红色值均不变;4) Degumming: Centrifuge the crude tea seed oil to remove the sediment, measure the acid value to 1.80mgKOH/g, then keep the temperature of the crude camellia seed oil at 30°C, add 1% degummed solid of the crude camellia seed oil for adsorption agent, the treatment time is 0.3h, and then centrifuged to obtain the degummed tea seed oil, and the heating test analysis is carried out. The analysis result is that there is no precipitate, and the yellow value and red value are unchanged;
5)脱酸:将脱胶茶籽油的温度保持在30℃,加入脱胶茶籽油质量1.6%的脱酸固体吸附剂,处理时间为1h,接着离心分离获得油脂(天然原生态油脂,或称脱酸茶籽油),测定酸值为0.19mgKOH/g,中性油得率为97.2%。5) Deacidification: keep the temperature of the degummed tea seed oil at 30°C, add a deacidified solid adsorbent with a quality of 1.6% of the degummed tea seed oil, and process for 1 hour, then centrifuge to obtain oil (natural original ecological oil, or Deacidified tea seed oil), the measured acid value is 0.19mgKOH/g, and the yield of neutral oil is 97.2%.
所述的脱胶固体吸附剂由①膨润土,②硅酸盐,③二氧化硅,④磷酸四种原料制备而成,各原料所占质量百分数为:膨润土:30%,硅酸盐:50%,二氧化硅:17%,磷酸:3%。The degummed solid adsorbent is prepared from four raw materials: ① bentonite, ② silicate, ③ silicon dioxide, and ④ phosphoric acid. The mass percentages of each raw material are: bentonite: 30%, silicate: 50%, Silica: 17%, Phosphoric Acid: 3%.
其制备方法为:将膨润土、硅酸盐、二氧化硅分别进行干燥处理,然后分别粉碎处理,粗细粒度为20目;然后将膨润土、硅酸盐和二氧化硅与磷酸进行均匀混合,即获得脱胶固体吸附剂。Its preparation method is as follows: dry bentonite, silicate and silicon dioxide respectively, and then pulverize them separately, with a particle size of 20 meshes; then uniformly mix bentonite, silicate and silicon dioxide with phosphoric acid to obtain Degummed solid sorbent.
所述的脱酸固体吸附剂由碱性化合物和油料作物种籽壳原料制备而成,各原料所占质量百分数为:碱性化合物10%,油料作物种籽壳90%;所述的油料作物种籽壳为葵花籽壳;所述的碱性化合物为氢氧化钙;The deacidification solid adsorbent is prepared from basic compounds and oil crop seed shell raw materials, and the mass percentage of each raw material is: basic compound 10%, oil crop seed shell 90%; the oil crop The seed shell is sunflower seed shell; the basic compound is calcium hydroxide;
其制备方法:Its preparation method:
1)原料选取:按上述选取;1) Raw material selection: select as above;
2)活化:将油料作物种籽壳进行清理,然后在60℃条件下干燥1h,再在500℃条件下活化1h,获得活化物;2) Activation: cleaning the seed shells of oil crops, drying at 60°C for 1 hour, and then activating at 500°C for 1 hour to obtain the activated product;
3)粉碎:将活化物粉碎至20目;3) Pulverization: pulverize the active substance to 20 meshes;
4)吸附:将碱性化合物配制成浓度为5wt%含碱性化合物的水溶液,将粉碎后的活化物置于容器中,加入含碱性化合物的水溶液,在20℃下搅拌0.5h;搅拌后过滤,分离出固体物;4) Adsorption: prepare the basic compound into a 5wt% aqueous solution containing the basic compound, put the pulverized active substance in a container, add the aqueous solution containing the basic compound, stir at 20°C for 0.5h; filter after stirring , to separate the solids;
5)干燥:将固体物进行干燥,得到脱酸固体吸附剂。5) Drying: drying the solid matter to obtain a deacidified solid adsorbent.
实施例4:Example 4:
如图1所示,一种油脂低温制取的方法,它包括如下步骤:As shown in Figure 1, a kind of method for oil and fat low temperature preparation, it comprises the steps:
1)清理:以葵花籽为原料,除去油料杂质;1) Cleaning: use sunflower seeds as raw materials to remove oil impurities;
2)调质:调节葵花籽的温度和水分,调质后的葵花籽温度为5℃,葵花籽的质量含水量调节到4%;2) Tempering: adjust the temperature and moisture of the sunflower seeds, the temperature of the sunflower seeds after conditioning is 5°C, and the mass water content of the sunflower seeds is adjusted to 4%;
3)低温压榨:将调质后的葵花籽进行压榨,葵花籽的入榨温度为-10℃,入榨葵花籽的质量含水量为4%,获得毛油;3) Low-temperature pressing: pressing the conditioned sunflower seeds, the temperature of the sunflower seeds for pressing is -10°C, and the mass water content of the sunflower seeds for pressing is 4%, to obtain crude oil;
4)脱胶:将毛油温度保持在5℃,加入脱胶固体吸附剂,脱胶固体吸附剂的添加量为毛油质量的0.1%,脱胶时间为0.1h;4) Degumming: keep the temperature of the crude oil at 5°C, add a degumming solid adsorbent, the amount of the degumming solid adsorbent is 0.1% of the mass of the crude oil, and the degumming time is 0.1h;
5)脱酸:将脱胶后的毛油温度保持在5℃,加入脱酸固体吸附剂,脱酸固体吸附剂的添加量为脱胶后毛油质量的0.1%,脱酸时间为0.1h,得到油脂(天然原生态油脂)。5) Deacidification: keep the temperature of the degummed crude oil at 5°C, add a deacidification solid adsorbent, the amount of the deacidification solid adsorbent is 0.1% of the mass of the degummed crude oil, and the deacidification time is 0.1h, to obtain Oil (natural raw oil).
所述的脱胶固体吸附剂由①膨润土,②硅酸盐,③二氧化硅,④磷酸四种原料制备而成,各原料所占质量百分数为:膨润土:60%,硅酸盐:20%,二氧化硅:19.9%,磷酸:0.1%。The degummed solid adsorbent is prepared from four raw materials: ① bentonite, ② silicate, ③ silicon dioxide, and ④ phosphoric acid. The mass percentages of each raw material are: bentonite: 60%, silicate: 20%, Silica: 19.9%, phosphoric acid: 0.1%.
其制备方法为:将膨润土、硅酸盐、二氧化硅分别进行干燥处理,然后分别粉碎处理,粗细粒度为200目;然后将膨润土、硅酸盐和二氧化硅与磷酸进行均匀混合,即获得脱胶固体吸附剂。The preparation method is as follows: drying bentonite, silicate and silicon dioxide respectively, and then pulverizing them respectively, with a particle size of 200 meshes; then uniformly mixing bentonite, silicate and silicon dioxide with phosphoric acid to obtain Degummed solid sorbent.
所述的脱酸固体吸附剂由碱性化合物和油料作物种籽壳原料制备而成,各原料所占质量百分数为:碱性化合物2%,油料作物种籽壳98%;所述的油料作物种籽壳为蓖麻壳和核桃壳的混合,蓖麻壳、核桃壳各占油料作物种籽壳总质量的50%;所述的碱性化合物为碳酸钠和碳酸钾的混合,碳酸钠、碳酸钾各占碱性化合物总质量的50%;The deacidification solid adsorbent is prepared from basic compounds and oil crop seed shell raw materials, and the mass percentage of each raw material is: 2% of basic compound, 98% of oil crop seed shell; the oil crop The seed shell is the mixture of castor bean shell and walnut shell, each of castor bean shell and walnut shell accounts for 50% of the total mass of the oil crop seed shell; the basic compound is the mixture of sodium carbonate and potassium carbonate, sodium carbonate, Potassium carbonate each accounts for 50% of the total mass of alkaline compounds;
其制备方法:Its preparation method:
1)原料选取:按上述选取;1) Raw material selection: select as above;
2)活化:将油料作物种籽壳进行清理,然后在60℃条件下干燥1h,再在150℃条件下活化1h,获得活化物;2) Activation: cleaning the seed shells of oil crops, drying at 60°C for 1 hour, and then activating at 150°C for 1 hour to obtain the activated product;
3)粉碎:将活化物粉碎至20目;3) Pulverization: pulverize the active substance to 20 mesh;
4)吸附:将碱性化合物配制成浓度为5wt%含碱性化合物的水溶液,将粉碎后的活化物置于容器中,加入含碱性化合物的水溶液,在20℃下搅拌0.5h;搅拌后过滤,分离出固体物;4) Adsorption: prepare the basic compound into a 5wt% aqueous solution containing the basic compound, put the pulverized active substance in a container, add the aqueous solution containing the basic compound, stir at 20°C for 0.5h; filter after stirring , to separate the solids;
5)干燥:将固体物进行干燥,得到脱酸固体吸附剂。5) Drying: drying the solid matter to obtain a deacidified solid adsorbent.
实施例5:Example 5:
如图1所示,一种油脂低温制取的方法,它包括如下步骤:As shown in Figure 1, a kind of method for oil and fat low temperature preparation, it comprises the steps:
1)清理:以葵花籽为原料,除去油料杂质;1) Cleaning: use sunflower seeds as raw materials to remove oil impurities;
2)调质:调节葵花籽的温度和水分,调质后的葵花籽温度为65℃,葵花籽的质量含水量调节到16%;2) Tempering: adjust the temperature and moisture of the sunflower seeds, the temperature of the sunflower seeds after conditioning is 65°C, and the mass water content of the sunflower seeds is adjusted to 16%;
3)低温压榨:将调质后的葵花籽进行压榨,葵花籽的入榨温度为65℃,入榨葵花籽的质量含水量为16%,获得毛油;3) Low-temperature pressing: pressing the conditioned sunflower seeds, the sunflower seeds are pressed at a temperature of 65° C., and the mass water content of the sunflower seeds to be pressed is 16%, to obtain crude oil;
4)脱胶:将毛油温度保持在65℃,加入脱胶固体吸附剂,脱胶固体吸附剂的添加量为毛油质量的5%,脱胶时间为2h;4) Degumming: keep the crude oil temperature at 65°C, add a degumming solid adsorbent, the amount of the degumming solid adsorbent is 5% of the crude oil mass, and the degumming time is 2h;
5)脱酸:将脱胶后的毛油温度保持在65℃,加入脱酸固体吸附剂,脱酸固体吸附剂的添加量为脱胶后毛油质量的2%,脱酸时间为3h,得到油脂(天然原生态油脂)。5) Deacidification: keep the temperature of the degummed crude oil at 65° C., add a deacidification solid adsorbent, the amount of the deacidification solid adsorbent is 2% of the mass of the degummed crude oil, and the deacidification time is 3 hours to obtain oil (natural raw oil).
所述的脱胶固体吸附剂由①膨润土,②硅酸盐,③二氧化硅,④柠檬酸四种原料制备而成,各原料所占质量百分数为:膨润土:30%,硅酸盐:27%,二氧化硅:40%,柠檬酸:3%;The degummed solid adsorbent is prepared from four raw materials: ① bentonite, ② silicate, ③ silicon dioxide, and ④ citric acid. The mass percentages of each raw material are: bentonite: 30%, silicate: 27% , silicon dioxide: 40%, citric acid: 3%;
其制备方法为:Its preparation method is:
将膨润土、硅酸盐、二氧化硅分别进行干燥处理,然后分别粉碎处理,粗细粒度为200目;然后将膨润土、硅酸盐和二氧化硅与柠檬酸进行均匀混合,即获得脱胶固体吸附剂。Dry bentonite, silicate, and silicon dioxide separately, and then pulverize them separately, with a particle size of 200 meshes; then uniformly mix bentonite, silicate, silicon dioxide and citric acid to obtain a degummed solid adsorbent .
所述的脱酸固体吸附剂由碱性化合物和油料作物种籽壳原料制备而成,各原料所占质量百分数为:碱性化合物35%,油料作物种籽壳98%;所述的油料作物种籽壳为葵花籽壳;所述的碱性化合物为碳酸钠;The deacidification solid adsorbent is prepared from basic compounds and oil crop seed shell raw materials, and the mass percentage of each raw material is: basic compound 35%, oil crop seed shell 98%; the oil crop The seed shell is sunflower seed shell; the basic compound is sodium carbonate;
所述的脱酸固体吸附剂的制备方法:The preparation method of described deacidification solid adsorbent:
1)原料选取:按上述选取;1) Raw material selection: select as above;
2)活化:将油料作物种籽壳进行清理,然后在110℃条件下干燥3h,再在500℃条件下活化7h,获得活化物;2) Activation: Clean the seed shells of oil crops, then dry them at 110°C for 3 hours, and then activate them at 500°C for 7 hours to obtain activated products;
3)粉碎:将活化物粉碎至100目;3) Pulverization: pulverize the active substance to 100 mesh;
4)吸附:将碱性化合物配制成浓度为45wt%含碱性化合物的水溶液,将粉碎后的活化物置于容器中,加入含碱性化合物的水溶液,在80℃下搅拌5h;搅拌后过滤,分离出固体物;4) Adsorption: prepare the basic compound into an aqueous solution containing a basic compound with a concentration of 45 wt%, place the pulverized active substance in a container, add the aqueous solution containing a basic compound, and stir for 5 hours at 80° C.; filter after stirring, solids are separated;
5)干燥:将固体物进行干燥,得到脱酸固体吸附剂。5) Drying: drying the solid matter to obtain a deacidified solid adsorbent.
本发明所列举的各原料,以及本发明各原料的上下限、区间取值,以及工艺参数(如温度、时间等)的上下限、区间取值都能实现本发明,在此不一一列举实施例。Each raw material enumerated in the present invention, and the upper and lower limits of each raw material of the present invention, the interval value, and the upper and lower limits of process parameters (such as temperature, time, etc.), the interval value can realize the present invention, do not enumerate one by one here Example.
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