阅读说明：本技术 一种生物基防冻剂的制备方法 (Preparation method of bio-based anti-freezing agent ) 是由 张龙 汤婉婷 于 2021-09-24 设计创作，主要内容包括：本发明一种生物基防冻剂的制备方法,采用高效催化液化技术,催化液化生物质原料制备环保防冻介质,属于化工材料生物质高效利用技术领域。以农业废弃物为原料,去离子水为液化剂,甲酸为催化剂,催化液化反应一定时间后,冷却,加氢氧化钾中和至pH7.0-8.0,过滤,得到的液体产物即为生物基防冻剂。所得防冻介质的冰点在-40℃,沸点为118-120℃,产品收率95%以上。所得介质无毒无害,对各种金属材料及高分子材料无腐蚀作用,可应用于工业冷却介质、防冻介质及道路融雪剂等。(The invention relates to a preparation method of a bio-based antifreeze, which adopts an efficient catalytic liquefaction technology to catalytically liquefy biomass raw materials to prepare an environment-friendly antifreeze medium, and belongs to the technical field of efficient utilization of chemical material biomass. The method comprises the steps of taking agricultural wastes as raw materials, deionized water as a liquefying agent and formic acid as a catalyst, carrying out catalytic liquefaction reaction for a certain time, cooling, adding potassium hydroxide for neutralization until the pH value is 7.0-8.0, and filtering to obtain a liquid product, namely the bio-based antifreeze. The freezing point of the obtained antifreezing medium is-40 ℃, the boiling point is 118-120 ℃, and the product yield is more than 95%. The obtained medium is nontoxic and harmless, has no corrosion effect on various metal materials and high polymer materials, and can be applied to industrial cooling media, antifreezing media, road snow melting agents and the like.)

1. A preparation method of a bio-based antifreeze comprises the following steps: adding a certain mass of biomass raw material into a 10L stainless steel reaction kettle provided with a stirring device and a temperature control device, then adding 1-2 times of liquefying agent and catalyst which accounts for 5.0-15.0% of the total mass of the liquefying raw material and the liquefying agent into the reaction kettle, uniformly mixing, reacting for 6-12h at the temperature of 110 plus 140 ℃, cooling the liquefied product to room temperature, performing centrifugal separation, and adding potassium hydroxide into the liquid product to adjust the pH value to 7.0-8.0, thus obtaining the bio-based antifreeze.

2. The method for preparing a bio-based anti-freezing agent according to claim, wherein the method comprises the following steps: the method adopts an efficient catalytic liquefaction technology, and the raw materials are various plant straw powder with the granularity of 80-100 meshes.

3. The method for preparing a bio-based anti-freezing agent according to claim, wherein the method comprises the following steps: the liquefying agent is deionized water, and the mass ratio of the liquefying agent to the raw materials is 1-2: 1.

4. The method for preparing a bio-based anti-freezing agent according to claim, wherein the method comprises the following steps: the catalyst is formic acid, and the mass of the added catalyst is 5.0-15.0% of the total mass of the liquefaction raw material and the liquefaction agent.

5. The method for preparing a bio-based anti-freezing agent according to claim, wherein the method comprises the following steps: the catalytic liquefaction reaction temperature is 110-140 ℃, and the reaction time is 6-12 h.

6. The method for preparing a bio-based antifreeze according to any one of claims 1 to 5, which comprises the steps of: it is suitable for industrial antifreezing medium, cooling medium and road snow-melting agent.

Technical Field

The invention relates to the technical field of high-quality utilization of new chemical materials and biomass, in particular to a preparation method and application of a biomass-based antifreezing medium.

Background

The glycol type antifreezing solution is an antifreezing product widely used in industry, but because glycol has higher cost and certain biotoxicity and does not conform to the concept of green products, the application field of the product is continuously limited, and under the condition, the environment-friendly antifreezing medium obtains more and more attention in industry. At present, the types of the antifreezing media include glycerol type antifreezing solution, polyethylene glycol type antifreezing solution and the like.

The biomass-based antifreezing medium mainly comprises biomass components such as polyhydric alcohol and the like, is non-toxic and harmless, has no negative effect on the environment after subsequent treatment, and does not corrode metal and organic high polymer materials. Therefore, the product is not only environment-friendly, but also reduces the subsequent treatment cost, so the antifreezing medium has more practical application value.

Disclosure of Invention

Aiming at the problems, the invention provides a method for preparing an antifreezing medium by catalytic liquefaction of agricultural wastes, which has the characteristics of low freezing point and high boiling point, has good corrosion resistance, does not need to add any corrosion inhibitor, and has the advantages of simple process operation, low price, environmental protection and the like. In order to achieve the above object, the present invention adopts the following technical solutions:

a preparation method of a bio-based antifreeze agent adopts an efficient catalytic liquefaction technology, agricultural and forestry waste raw materials, a liquefying agent and a catalyst are sequentially added into a reaction device according to a certain proportion, after uniform mixing, reaction is carried out for 6-12h under the condition of 110-140 ℃, after cooling, potassium hydroxide is added to adjust the pH value to 7.5-8.0, and filtration is carried out, so that the obtained liquid product is the bio-based antifreeze agent.

The raw materials are various straw powders with the granularity of 80-100 meshes.

The mass ratio of the raw material to the liquefying agent is 1-1.5: 1.

The reaction temperature is 110-140 ℃, and the preferable temperature is 120-130 ℃.

The reaction time is 6-12h, preferably 7-10 h.

The catalyst is formic acid, and the addition amount of the catalyst is 5.0-15.0% of the total mass of the liquefying agent and the raw materials. Preferably 8.0% to 12.0%.

Due to the adoption of the technical scheme, the invention has the beneficial effects that:

(1) the invention adopts the high-efficiency catalytic liquefaction technology, compared with the common liquefaction technology, the high-efficiency liquefaction of the raw materials can be realized, the liquefaction product obtained by optimizing the components of the formula has low freezing point and weak corrosivity on metals, the technological process is simple to operate, and the cost is greatly reduced. (2) The liquefied product of the invention mainly takes biomasses such as polyalcohol and the like as main components, is environment-friendly and nontoxic, and compared with the traditional glycol type antifreezing medium, the cost of the treatment of the waste antifreezing medium is reduced, and the harm to the environment of an ecosystem is greatly reduced.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.

Example 1.

Sequentially adding 2.0Kg of corn straw powder, 2.0Kg of deionized water and 0.62Kg of formic acid into a 10L stainless steel reactor provided with a stirring device and a temperature control device, uniformly stirring, controlling the temperature of the reactor to 120 ℃, reacting for 5 hours, rapidly cooling to room temperature, centrifuging, adding 0.75Kg of potassium hydroxide into the obtained liquefied product, adjusting the pH to 7.7, and obtaining the biomass-based antifreezing medium, wherein the product yield is 92.3%, the freezing point is-41 ℃, and the boiling point is 120 ℃.

Example 2.

2.0Kg of wheat straw powder, and,

3.0Kg of deionized water and 0.5Kg of formic acid are uniformly stirred, the temperature of the reactor is controlled to 140 ℃ for 8 hours of reaction, the reactor is cooled to room temperature and then centrifuged, the liquefied product is adjusted to pH 7.7 by potassium hydroxide to obtain the biomass-based antifreezing medium, and the yield of the product is 93.4 percent, the freezing point is-40 ℃ and the boiling point is 118 ℃ through determination.

Example 3.

Adding 5.0kg of straw powder, 5.0kg of deionized water and 1.55kg of formic acid into a 10L stainless steel reaction kettle provided with a stirring device and a temperature control device in sequence, stirring uniformly, reacting at 130 ℃ for 10h, cooling to room temperature, centrifuging, adjusting the pH of the obtained liquefied product to 7.9 by using potassium hydroxide to obtain a biomass-based antifreezing medium, and determining that the yield of the product is 90.2%, the freezing point is-41 ℃ and the boiling point is 118 ℃.

EXAMPLE 4 preparation of antifreeze media from liquefied products

Note: the indexes are all superior to the national standard (GB 29743-

EXAMPLE 5 preparation of snow-melting Agents from liquefied products

Note: the indexes are all superior to the national standard (GB 29743-

The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing examples can be modified, or some technical features can be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions.