阅读说明：本技术 一种制备相变蜡的方法 (Method for preparing phase-change wax ) 是由 张硕鹏 吴俊岭 张建雨 于 2021-07-23 设计创作，主要内容包括：本发明公开了一种制备相变蜡的方法,本发明涉及相变蜡制备技术领域。通过加入结晶添加剂,可在发汗原料冷却过程中起到了成核、吸附和共晶的作用,有利于油分从晶体之间流出,从而有利于发汗过程的进行,大大提高了发汗效率和提高了发汗产品质量,降低了产品含油量,提高了产品熔点,进一步增加了产品石蜡的收率,具有成本低、效益好等优点,同时还可多次发汗制备相变材料,在发汗过程中第一次加热发汗则为拔头发汗脱油,主要的作用,是达到去除大部分原料中的油分,节约发汗时间,提高发汗效率的效果,而二次或多次发汗工艺,则有利于提高产品收率和产品质量,主要起到提高发汗脱油率的作用,进一步降低了产品含油的效果。(The invention discloses a method for preparing phase-change wax, and relates to the technical field of phase-change wax preparation. By adding the crystallization additive, the crystallization additive can play the roles of nucleation, adsorption and eutectic crystallization in the cooling process of the sweating raw material, is beneficial to the oil component to flow out from the crystals, thereby being beneficial to the sweating process, greatly improving the sweating efficiency and the sweating product quality, reducing the oil content of the product, improving the melting point of the product, further increasing the yield of the paraffin wax of the product, having the advantages of low cost, good benefit and the like, and simultaneously being capable of sweating for multiple times to prepare the phase-change material, the first heating sweating in the sweating process is head-drawing sweating deoiling, has the main functions of removing oil in most raw materials, saving sweating time and improving sweating efficiency, and the secondary or multiple sweating process is beneficial to improving the product yield and the product quality, mainly plays a role in improving the sweating deoiling rate and further reduces the oil-containing effect of the product.)

1. A method of making a phase change wax comprising the steps of:

s1, preparing materials: weighing raw wax and crystallization additive according to a proportion and placing the raw wax and the crystallization additive aside for later use;

s2, water filling: adding water cushion to the bottom of the sweating dish to fill the space below the sieve plate;

s3, charging: putting the raw material wax prepared in the S1 and the crystallization additive into a reaction kettle together, heating to a temperature above a melting point, starting a stirrer to mix uniformly when the raw material wax and the crystallization additive are in a liquid state, and adding the mixture into a sweating dish;

s4, cooling: when the temperature of the raw material wax reaches 10-20 ℃ below the melting point of the raw material, the pad water in the sweating dish can be discharged;

s5, heating: starting an electric heating system, and heating the sweating dish at the speed of 0.5-2 ℃/h to slowly heat the raw material wax;

s6, preparing and forming: and (5) after the heating in the step S5 is finished, when the temperature of the sweating box reaches 2 ℃ above the melting point of the raw materials, namely the temperature of the sweating box is 50-80 ℃, keeping the constant temperature for 2 hours, and taking out the materials remained after sweating in the sweating dish to obtain the crude wax of the intermediate product.

S7, repeated sweating: and (3) repeating the operations of the step S2, the step S3, the step S4 and the step S5 by using the intermediate product crude wax obtained in the step S6, wherein the cooling temperature in the step S4 is 10-20 ℃ below the melting point of the raw material, the heating rate in the step S5 is 1 ℃/hour, the heating final temperature is 3-10 ℃ above the melting point of the raw material, and the intermediate product crude wax is slowly heated, so that repeated sweating operation can be finished finally, and a finer sweating product is obtained.

3. The method of claim 1, wherein the melting point of the raw material wax in step S3 is 48-78 ℃ and the oil content is 0.5-12%.

4. The method of claim 1, wherein the cooling rate in step S4 is 0.5-10 ℃/h, and the electric heating system in step S5 is an electric heating box, and the cooling rate is 0.5-4 ℃/h.

5. The method of claim 1, wherein the raw wax and the crystallization additive are present in the following amounts by weight: 15.0-25.0 kg of raw wax and 0.05-0.15 kg of crystallization additive.

6. The method of claim 4, wherein the raw wax and the crystallization additive are present in the following amounts by weight: 15.0 kg of raw wax and 0.05 kg of crystallization additive.

7. The method of claim 4, wherein the raw wax and the crystallization additive are present in the following amounts by weight: 20.0 kg of raw wax and 0.1 kg of crystallization additive.

8. The method of claim 4, wherein the raw wax and the crystallization additive are present in the following amounts by weight: 25.0 kg of raw wax and 0.15 kg of crystallization additive.

9. The method of claim 4, wherein the crystallization additive is one or more of calcium alkyl salicylate, ethylene-vinyl acetate copolymer, and alkyl naphthalene condensate.

10. The method of claim 1, wherein the sweating in step S7 is repeated for an unlimited number of times.

Technical Field

The invention relates to the technical field of phase-change wax preparation, in particular to a method for preparing phase-change wax.

Background

The main performance indicators of phase change waxes are the melting point and enthalpy of the phase change wax. The melting point of the phase-change wax is proper, the melting range of the phase-change wax is required to be small besides the melting point required by customers, if the melting range of the phase-change wax is large, the useful phase-change heat quantity in practical application of the phase-change wax is reduced, in this case, even if the total phase-change heat is very large, the user requirement cannot be met, and particularly in the high-end application fields of the phase-change wax such as electronic components, chips and the like, the melting range of the phase-change wax is required to be smaller and better. In addition, the enthalpy value and the melting range of the phase-change wax are seriously influenced by the oil content of the phase-change wax, the smaller the oil content of the phase-change wax is, the larger the enthalpy value of the phase-change wax is, the smaller the melting range of the phase-change wax is, because the oil content of the phase-change wax reduces the enthalpy value of the phase-change wax and increases the melting range of the phase-change wax.

The sweating deoiling is one of the important means commonly used for producing various low oil-containing paraffin. However, the research on adding the sweating raw material crystallization additive in the sweating process is blank, if the crystallization additive capable of increasing the wax component crystallization crystal is added in the sweating deoiling process, the oil in the sweating raw material can smoothly flow out in the sweating process, so that the oil content of a sweating product is reduced, the enthalpy value of the phase-change wax is increased, the melting range of the phase-change wax is reduced, and the sweating efficiency is improved.

Disclosure of Invention

Aiming at the defects of the prior art, the invention provides a method for preparing phase-change wax, which solves the problems of low sweating deoiling outflow speed, high oil content of product wax, low enthalpy value of the product and low yield of product paraffin.

In order to achieve the purpose, the invention is realized by the following technical scheme: a method of making a phase change wax comprising the steps of:

s1, preparing materials: weighing raw wax and crystallization additive according to a proportion and placing the raw wax and the crystallization additive aside for later use;

s2, water filling: adding water cushion to the bottom of the sweating dish to fill the space below the sieve plate;

s3, charging: putting the raw material wax prepared in the S1 and the crystallization additive into a reaction kettle together, heating to a temperature above a melting point, starting a stirrer to mix uniformly when the raw material wax and the crystallization additive are in a liquid state, and adding the mixture into a sweating dish;

s4, cooling: when the temperature of the raw material wax reaches 10-20 ℃ below the melting point of the raw material, the pad water in the sweating dish can be discharged;

s5, heating: starting an electric heating system, and heating the sweating dish at the speed of 0.5-2 ℃/h to slowly heat the raw material wax;

s6, preparing and forming: and (5) after the heating in the step S5 is finished, when the temperature of the sweating box reaches 2 ℃ above the melting point of the raw materials, namely the temperature of the sweating box is 50-80 ℃, keeping the constant temperature for 2 hours, and taking out the materials remained after sweating in the sweating dish to obtain the crude wax of the intermediate product.

S7, repeated sweating: and (3) repeating the operations of the step S2, the step S3, the step S4 and the step S5 by using the intermediate product crude wax obtained in the step S6, wherein the cooling temperature in the step S4 is 10-20 ℃ below the melting point of the raw material, the heating rate in the step S5 is 1 ℃/hour, the heating final temperature is 3-10 ℃ above the melting point of the raw material, and the intermediate product crude wax is slowly heated, so that repeated sweating operation can be finished finally, and a finer sweating product is obtained.

As a further technical scheme of the invention, the melting point of the raw material wax in the step S3 is 48-78 ℃, and the oil content is 0.5-12%.

As a further technical scheme of the invention, the cooling rate in the step S4 is 0.5-10 ℃/h, and the electric heating system in the step S5 is an electric heating box, and the cooling rate is 0.5-4 ℃/h.

As a further technical scheme of the invention, the raw material wax and the crystallization additive comprise the following components in parts by weight: 15.0-25.0 kg of raw wax and 0.05-0.15 kg of crystallization additive.

As a further technical scheme of the invention, the raw material wax and the crystallization additive comprise the following components in parts by weight: 15.0 kg of raw wax and 0.05 kg of crystallization additive.

As a further technical scheme of the invention, the raw material wax and the crystallization additive comprise the following components in parts by weight: 20.0 kg of raw wax and 0.1 kg of crystallization additive.

As a further technical scheme of the invention, the raw material wax and the crystallization additive comprise the following components in parts by weight: 25.0 kg of raw wax and 0.15 kg of crystallization additive.

As a further technical scheme of the invention, the crystallization additive is one or more of calcium alkyl salicylate, ethylene-vinyl acetate copolymer and alkyl naphthalene condensate.

As a further technical solution of the present invention, the number of times of repeating sweating in the step S7 is not limited.

Advantageous effects

The invention provides a method for preparing phase-change wax. Compared with the prior art, the method has the following beneficial effects:

1. a method for preparing phase-change wax, through adding crystalline additive, can play the effects of nucleation, absorption and eutectic crystal in the cooling process of raw materials of sweating, have formed the large flake paraffin crystallization finally, the space is great between the crystal, help the oil content to flow out from between the crystal while sweating, thus help the going on of the sweating process, has greatly raised the sweating efficiency and improved the quality of sweating product, has reduced the oil content of the product, has raised the melting point of the product, has further increased the yield of the product paraffin, have advantages such as being simple and easy, with low costs, good benefits.

2. The first heating sweating is head drawing sweating deoiling, which is mainly to remove oil in most raw materials, save sweating time and improve sweating efficiency, while the second heating or repeated heating sweating is fine sweating which mainly plays a role in improving sweating deoiling rate and further reduces the oil content of the product.

Drawings

FIG. 1 is a flow chart of the preparation method of the present invention.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1

The invention provides a technical scheme that: a method of making a phase change wax comprising the steps of:

s1, preparing materials: weighing raw wax and crystallization additive according to a proportion and placing the raw wax and the crystallization additive aside for later use;

s2, water filling: adding water cushion to the bottom of the sweating dish to fill the space below the sieve plate;

s3, charging: putting the raw material wax prepared in the S1 and the crystallization additive into a reaction kettle together, heating to a temperature above a melting point, starting a stirrer to mix uniformly when the raw material wax and the crystallization additive are in a liquid state, and adding the mixture into a sweating dish;

s4, cooling: when the temperature of the raw material wax reaches 10 ℃ below the melting point of the raw material, the pad water in the sweating dish can be discharged;

s5, heating: starting an electric heating system, and heating the sweating dish at the speed of 0.5 ℃/h to slowly heat the raw material wax;

s6, intermediate product crude wax: after the heating in the step S5 is finished, when the temperature of the sweating box reaches 2 ℃ above the melting point of the raw materials, namely the temperature of the sweating box is 50 ℃, keeping the temperature for 2 hours, and taking out the materials remained after sweating in the sweating dish to obtain an intermediate product crude wax;

s7, repeated sweating: and (4) repeating the operations of the step S2, the step S3, the step S4 and the step S5 by using the intermediate product crude wax obtained in the step S6, wherein the cooling temperature in the step S4 is 10 ℃, the heating rate in the step S5 is 1 ℃/hour, the heating final temperature is 3 ℃, the intermediate product crude wax is slowly heated, and finally, the repeated sweating operation can be completed to obtain a finer sweating product.

The melting point of the raw material wax in the step S3 is 48 ℃, and the oil content is 0.5%;

the cooling rate in the step S4 is 0.5 ℃/h, the electric heating system in the step S5 is an electric heating box, and the cooling rate is 0.5 ℃/h;

in this embodiment, the raw material wax and the crystallization additive are in parts by weight: 15.0 kg of raw wax and 0.05 kg of crystallization additive;

the crystallization additive is calcium alkyl salicylate.

The number of repetitions of sweating in step S7 is not limited.

Example 2

The invention provides a technical scheme that: a method of making a phase change wax comprising the steps of:

s1, preparing materials: weighing raw wax and crystallization additive according to a proportion and placing the raw wax and the crystallization additive aside for later use;

s2, water filling: adding water cushion to the bottom of the sweating dish to fill the space below the sieve plate;

s3, charging: putting the raw material wax prepared in the S1 and the crystallization additive into a reaction kettle together, heating to a temperature above a melting point, starting a stirrer to mix uniformly when the raw material wax and the crystallization additive are in a liquid state, and adding the mixture into a sweating dish;

s4, cooling: when the temperature of the raw material wax reaches 15 ℃ below the melting point of the raw material, the pad water in the sweating dish can be discharged;

s5, heating: starting an electric heating system, and heating the sweating dish at the speed of 1.8 ℃/h to slowly heat the raw material wax;

s6, intermediate product crude wax: after the heating in the step S5 is finished, when the temperature of the sweating box reaches 2 ℃ above the melting point of the raw materials, namely the temperature of the sweating box is 65 ℃, keeping the temperature for 2 hours, and taking out the materials remained after sweating in the sweating dish to obtain an intermediate product crude wax;

s7, repeated sweating: and (4) repeating the operations of the step S2, the step S3, the step S4 and the step S5 by using the intermediate product crude wax obtained in the step S6, wherein the cooling temperature in the step S4 is 15 ℃, the heating rate in the step S5 is 1 ℃/hour, the heating final temperature is 6 ℃, the intermediate product crude wax is slowly heated, and finally, the repeated sweating operation can be completed to obtain a finer sweating product.

The melting point of the raw material wax in the step S3 is 63 ℃, and the oil content is 6%;

the cooling rate in step S4 is 5 ℃/h, the electric heating system in step S5 is an electric heating box, and the cooling rate is 2.5 ℃/h;

in this embodiment, the raw material wax and the crystallization additive are in parts by weight: 20.0 kg of raw wax and 0.1 kg of crystallization additive;

the crystallization additive is an ethylene-vinyl acetate copolymer.

The number of repetitions of sweating in step S7 is not limited.

Example 3

The invention provides a technical scheme that: a method of making a phase change wax comprising the steps of:

s1, preparing materials: weighing raw wax and crystallization additive according to a proportion and placing the raw wax and the crystallization additive aside for later use;

s2, water filling: adding water cushion to the bottom of the sweating dish to fill the space below the sieve plate;

s3, charging: putting the raw material wax prepared in the S1 and the crystallization additive into a reaction kettle together, heating to a temperature above a melting point, starting a stirrer to mix uniformly when the raw material wax and the crystallization additive are in a liquid state, and adding the mixture into a sweating dish;

s4, cooling: when the temperature of the raw material wax reaches 20 ℃ below the melting point of the raw material, the pad water in the sweating dish can be discharged;

s5, heating: starting an electric heating system, and heating the sweating dish at the speed of 2 ℃/h to slowly heat the raw material wax;

s6, intermediate product crude wax: after the heating in the step S5 is finished, when the temperature of the sweating box reaches 2 ℃ above the melting point of the raw materials, namely the temperature of the sweating box is 80 ℃, keeping the temperature for 2 hours, and taking out the materials remained after sweating in the sweating dish to obtain an intermediate product crude wax;

s7, repeated sweating: and (4) repeating the operations of the step S2, the step S3, the step S4 and the step S5 by using the intermediate product crude wax obtained in the step S6, wherein the cooling temperature in the step S4 is 20 ℃, the heating rate in the step S5 is 1 ℃/hour, the heating final temperature is 10 ℃, the intermediate product crude wax is slowly heated, and finally, the repeated sweating operation can be completed to obtain a finer sweating product.

The melting point of the raw material wax in the step S3 ℃ is 78 ℃, and the oil content is 12%;

the cooling rate in step S4 is 5 ℃/h, the electric heating system in step S5 is an electric heating box, and the cooling rate is 4 ℃/h;

in this embodiment, the raw material wax and the crystallization additive are in parts by weight: 25.0 kg of raw wax and 0.15 kg of crystallization additive;

the crystallization additive is an alkyl naphthalene condensate.

The number of repetitions of sweating in step S7 is not limited.

There are three main classes that can be used as sweating crystallization additives: one is the ashless high polymers (polyolefins) such as: poly alpha-olefin, ethylene-propylene copolymer, alpha-olefin and CO copolymer and the like, which are all obtained by polymerization reaction of olefin monomers under certain conditions, wherein the effect key depends on the molecular weight distribution and average molecular weight of the polymer; polyesters including poly (toluene) acrylate, ethylene-vinyl acetate copolymers, copolymers of dialkyl fumarates and unsaturated esters, and the like; the effectiveness of such polymers depends on their average molecular weight, most critical being the carbon chain length of the ester-forming fatty alcohol;

alkyl naphthalene includes alkyl salicylate, sulfurized alkylphenol salt, aluminum salt of nitration distillate, alkyl sulfosalicylate, etc.;

and thirdly, the alkyl naphthalene condensate can be compounded with other polymer auxiliary agents for use, the alkyl chain length of the chlorinated paraffin is between C15 and C43, the chlorine content is 10 to 30 percent, when the length of the alkyl chain is the same as that of the carbon chain of the raw material oil wax, the best effect is achieved, and the average molecular weight of the alkyl naphthalene condensate is required to be more than 1000.

The melting point, enthalpy, phase-change wax yield and oil content of the product were measured according to the phase-change wax preparation composition of example 2 in different states of the crystalline additive, and the results are shown in the following table:

it is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.