CN217323924U

CN217323924U - Oxidized polyethylene wax production device

Info

Publication number: CN217323924U
Application number: CN202122344816.4U
Authority: CN
Inventors: 任海伦; 郝鹏鹏; 滕琳; 虞金霞
Original assignee: RENAI COLLEGE OF TIANJIN UNIVERSITY
Current assignee: RENAI COLLEGE OF TIANJIN UNIVERSITY
Priority date: 2021-09-27
Filing date: 2021-09-27
Publication date: 2022-08-30
Anticipated expiration: 2031-09-27

Abstract

The utility model belongs to the technical field of chemical oxidation reaction, in particular to a device for producing oxidized polyethylene wax, wherein an oxidation kettle comprises a first feed inlet, a second feed inlet and a discharge outlet; the polyethylene wax storage tank is connected with the first feeding hole through a pipeline, and polyethylene wax in the polyethylene wax storage tank is pumped into the oxidation kettle through a feeding pump; the hydrogen peroxide storage tank is connected with the second feed inlet through a pipeline, and hydrogen peroxide in the hydrogen peroxide storage tank is pumped into the oxidation kettle through a feed pump; polyethylene wax and hydrogen peroxide are oxidized in an oxidation kettle in a certain mass ratio under the action of a catalyst to carry out oxidation reaction. The utility model has the advantages that: polyethylene wax is stored in the polyethylene wax storage tank and is provided with reaction raw materials, hydrogen peroxide is stored in the hydrogen peroxide storage tank and is provided with an oxidant, and the oxidation kettle is used as a polyethylene wax and hydrogen peroxide reaction container to produce oxidized polyethylene wax, so that fire or explosion is not easy to occur, the reaction is mild, the controllability is high, the safety coefficient is high, the product color and luster are good, no pollution is caused, and the water content and the ash content are lower.

Description

Oxidized polyethylene wax production device

Technical Field

The utility model belongs to the technical field of chemical industry oxidation reaction, concretely relates to oxidation low molecular weight polyethylene's apparatus for producing.

Background

Polyolefins generally refer to a generic term for thermoplastic resins obtained by polymerizing or copolymerizing an α -olefin such as ethylene, propylene, 1-butene, 1-pentene, 1-hexene, 1-octene, 4-methyl-1-pentene, etc., and certain cyclic olefins, alone. The polyolefin with lower molecular weight is solid at normal temperature, has good chemical stability, dispersibility at high temperature, fluidity, impact resistance and lubricity, and plays a unique role in the chemical fields of plastics, rubber, printing ink, paint, metal casting and the like. Along with the development of production process and modified products, the application field of the modified products is continuously expanded, and the modified products become indispensable chemical raw materials in certain industries at present.

The polyethylene wax belongs to fine chemicals, and is modified, so that the physical and chemical properties of the polyethylene wax can be changed, the polyethylene wax has the performance characteristics suitable for specific process conditions, the application range and the effect of the polyethylene wax can be widened, and the additional value is improved. The oxidation is one of the polyethylene wax modification methods, the oxidized polyethylene wax is excellent novel polar wax, and the molecular chain of the oxidized polyethylene wax has a certain amount of carbonyl and hydroxyl, so that the compatibility with the filler, the pigment and the polar resin is obviously improved. The wettability and the dispersibility of the polyether polyol in a polar system are superior to those of polyethylene wax, and the polyether polyol also has coupling property. Oxidized Polyethylene Wax (OPW) has high utility value and is widely used in many fields. In order to adapt to the development and application of new technology and meet different requirements of various fields, various modification researches on polyethylene wax (PEW) are widely concerned.

The foreign oxidized polyethylene wax is developed rapidly, and the oxidized polyethylene wax varieties of some large-scale polyethylene wax manufacturers, such as Mitsui chemical company in Japan, Honeyville company in the United states and Pasteur company in Germany, are very abundant. In recent years, the study on oxidized polyethylene wax has been intensified in China, and researchers have studied the influence of various factors on the oxidation reaction by using carboxylate, zinc stearate, manganese sulfate, etc. as a catalyst and air as an oxidizing agent.

CN201910527722.5 provides a method for continuously synthesizing oxidized polyethylene wax, wherein a microchannel reactor or a packed tower is used as a reactor, and oxidizing gas and polyethylene wax are subjected to contact reaction on the surface of a packing to obtain oxidized polyethylene wax.

CN201720015346.8 provides a production device of oxidation polyethylene wax, including the reaction storehouse epitheca, the bottom edge connection of reaction storehouse epitheca has the ring flange, the bottom of reaction storehouse epitheca is connected with the reaction storehouse base through the ring flange, the inner chamber of reaction storehouse base is transversely installed and is supported the heat-conducting plate, the inner chamber of reaction storehouse base is provided with electric heating pipe, and electric heating pipe is located the bottom that supports the heat-conducting plate, this production device of oxidation polyethylene wax, through the setting of filter chamber, make the impurity in the material after the reaction filter, finally obtain oxidation polyethylene wax product.

CN201310288659.7 provides a preparation method of high-density oxidized polyethylene wax, which comprises the steps of carrying out thermal cracking on high-density polyethylene resin to obtain low-molecular-weight high-density polyethylene wax, dispersing the obtained high-density polyethylene wax in an aqueous medium by the aid of a dispersing agent in a pressure kettle at a temperature higher than the melting point of wax, introducing oxidizing gas at a temperature higher than the melting point of wax, oxidizing at a certain pressure, and finally washing and removing water to obtain the high-density oxidized polyethylene wax.

The oxidant in the process is air or oxygen, and is easy to cause fire or explosion; the product of the process or the device has the advantages of dark color, strong smell, high water content and ash content, and low safety coefficient of the device.

SUMMERY OF THE UTILITY MODEL

The utility model aims to overcome the defects in the prior art and provide a production device of oxidized polyethylene wax, which adopts hydrogen peroxide (H) ₂ O ₂ ) The oxidized polyethylene wax is an oxidant, and is not easy to cause fire or explosion; the product has good color and luster, no pollution, lower water content and ash content, mild reaction and high controllabilityAnd the safety coefficient of the device is high.

In order to achieve the aim, the utility model provides a device for producing oxidized polyethylene wax, which is characterized in that the device for producing oxidized polyethylene wax is characterized by comprising a polyethylene wax storage tank, an oxidation kettle and a hydrogen peroxide storage tank;

the oxidation kettle comprises a first feeding hole, a second feeding hole and a discharging hole; the first feeding hole and the second feeding hole are arranged at the upper part of one side of the oxidation kettle, and the discharge hole is arranged at the lowest discharge liquid level of the oxidation kettle;

the polyethylene wax storage tank is connected with the first feeding hole through a pipeline, and polyethylene wax in the polyethylene wax storage tank is pumped into the oxidation kettle through a feeding pump;

the hydrogen peroxide storage tank is connected with the second feed inlet through a pipeline, and hydrogen peroxide in the hydrogen peroxide storage tank is pumped into the oxidation kettle through a feed pump;

polyethylene wax and hydrogen peroxide are oxidized in an oxidation kettle to carry out oxidation reaction under the action of a catalyst according to a certain mass ratio, and a material flow c is discharged through a discharge hole.

Preferably, the system also comprises a heat exchanger and an oxidation kettle circulating pump, and the oxidation kettle also comprises a circulating port;

the circulation port is arranged on the upper portion of the other side of the oxidation kettle, the discharge port of the oxidation kettle is connected with the circulation port through a pipeline, an oxidation kettle circulating pump and a heat exchanger are arranged on the pipeline between the discharge port and the circulation port, the reaction temperature is controlled through the heat exchanger, the material flow c discharged from the discharge port enters the heat exchanger through the oxidation kettle circulating pump and then enters the oxidation kettle through the circulation port, the system pressure is passed after the reaction time is reached, and the material flow d is discharged from the discharge port of the oxidation kettle.

Preferably, the discharge port is provided with a regulating valve, and the discharge material flow d is regulated through an oxidation kettle discharge regulating valve of the discharge port.

Preferably, a stirring blade is arranged in the oxidation kettle, and the stirring speed of the stirring blade is as follows: 10-500 rpm, so that the polyethylene wax and the hydrogen peroxide are distributed more uniformly.

Preferably, the device also comprises a lightness-removing kettle, wherein the lightness-removing kettle comprises a lightness-removing feed inlet and a lightness-removing discharge outlet, the lightness-removing feed inlet is arranged at the middle upper part of one side of the lightness-removing kettle, and the lightness-removing discharge outlet is arranged at the lowest discharge liquid level of the lightness-removing kettle;

the discharge port of the oxidation kettle is connected with the light component removing kettle through a pipeline, a distribution port steam inlet pipe is arranged in the light component removing kettle, the material flow d enters the light component removing kettle, the light component removing kettle releases steam through the distribution port steam inlet pipe, the light component in the polyethylene wax is oxidized through steam stripping, the steam divides the greatly reduced light component, the light component in the oxidized polyethylene wax obtained through the reaction is removed, and the material flow g is obtained.

Preferably, the lightness-removing kettle further comprises a condensation port, the lightness-removing feed inlet is arranged at the upper part of the other side of the lightness-removing kettle, a condenser is arranged on a pipeline connected with the condensation port, and the removed material flow e is condensed by the condenser through the pipeline of the condensation port to obtain a material flow f.

Preferably, the device further comprises a dehydration kettle, wherein the dehydration kettle comprises a dehydration feed inlet, a dehydration discharge outlet and a vacuum port, the dehydration feed inlet is arranged at the middle upper part of one side of the dehydration kettle, the vacuum port is arranged at the upper part of the other side of the dehydration kettle, and the dehydration discharge outlet is arranged at the lowest discharge liquid level of the dehydration kettle;

a discharge port of the light component removal kettle is connected with a dehydration kettle through a pipeline, a vacuum port is connected with a negative pressure operation mechanism through a pipeline, a material flow g for removing light components enters the dehydration kettle, the vacuum degree of the dehydration kettle is controlled through the negative pressure operation mechanism, after operation is carried out for a period of time, a material flow i of an oxidized polyethylene wax product is obtained, and the material flow i is discharged by a discharge pump of the dehydration kettle to obtain a finished product oxidized polyethylene wax;

the negative pressure operating mechanism is a vacuum pump, and free water separated from the vacuum pump forms a material flow h.

Preferably, the reaction temperature of the oxidation kettle is 150-180 ℃.

Preferably, the temperature of saturated steam used in the lightness-removing kettle is 130-150 ℃, and the operating pressure of the lightness-removing kettle is 105-110 KPa.

Preferably, the operation temperature of the dehydration kettle is 120-150 ℃; the operation pressure of the dehydration kettle is 5-50 Kpa.

The utility model has the advantages that:

(1) the whole device has reasonable structure, is convenient to produce and high in safety coefficient, heat energy is effectively utilized, energy consumption is reduced, and light components of byproducts and free water are recycled;

(2) the polyethylene wax storage tank stores polyethylene wax to provide a reaction raw material, the hydrogen peroxide storage tank stores hydrogen peroxide to provide an oxidant, the oxidation kettle is used as a reaction container for producing oxidized polyethylene wax by using the polyethylene wax and the hydrogen peroxide, fire or explosion is not easy to occur, the reaction is mild, the reaction temperature is reduced, the controllability is high, the safety coefficient of the device is high, the light components produced by the product are fewer, the yield of the final product is high, the color and luster are good, no pollution is caused, the water content and the ash content are lower, and the acid value of the obtained oxidized polyethylene wax product is moderate;

(3) the light component removal process is carried out in a light component removal kettle, a steam feeding pipe with a distribution port is arranged in the light component removal kettle, and a steam stripping process is adopted, so that the partial pressure of light components is greatly reduced, the operating temperature is reduced, and the low odor of oxidized polyethylene wax is ensured;

(4) the dehydration process is carried out in the dehydration kettle, and the dehydration kettle is connected with the vacuum pump, adopts vacuum pump negative pressure operation, has reduced operating temperature, makes the desorption of the free water in the oxidation low molecular weight polyethylene thoroughly, has guaranteed the softening point of product.

Drawings

FIG. 1 is a schematic structural view of an apparatus for producing oxidized polyethylene wax according to example 1 of the present invention;

FIG. 2 is a schematic structural view of an apparatus for producing oxidized polyethylene wax according to embodiment 2 of the present invention;

FIG. 3 is a schematic structural view of an apparatus for producing oxidized polyethylene wax according to example 3 of the present invention;

FIG. 4 is a schematic structural view of an apparatus for producing oxidized polyethylene wax according to examples 4 and 5 of the present invention;

FIG. 5 is a process flow chart of a method for producing oxidized polyethylene wax by using an apparatus for producing oxidized polyethylene wax according to application example 2 of the present invention;

in the drawings: 1. a polyethylene wax storage tank; 2. a polyethylene wax feed pump; 3. a hydrogen peroxide storage tank; 4. a hydrogen peroxide feeding pump; 5. an oxidation kettle; 5-1, a first feed inlet; 5-2 parts of a second feeding hole and 5-3 parts of a circulating hole; 5-4, a discharge hole; 5-5, stirring leaves; 6. an oxidation kettle circulating pump; 7. a discharge regulating valve of the oxidation kettle; 8. A heat exchanger; 9. a light component removing kettle; 9-1, a light component removing feed inlet; 9-2, removing light materials; 9-3, a condensation port; 10. A distribution port steam feed pipe; 11. a condenser; 12. a dehydration kettle; 12-1, a dehydration feed inlet; 12-2, dewatering and discharging; 12-3, a vacuum port 13 and a vacuum pump; 14. a discharging pump of the dehydration kettle.

Detailed Description

The following describes the apparatus for producing oxidized polyethylene wax according to the present invention in detail with reference to the accompanying drawings.

A production device of oxidized polyethylene wax comprises a polyethylene wax storage tank, an oxidation kettle and a hydrogen peroxide storage tank;

the oxidation kettle comprises a first feeding hole, a second feeding hole and a discharging hole; the first feeding hole and the second feeding hole are arranged at the upper part of one side of the oxidation kettle, and the discharge hole is arranged at the lowest liquid discharge level of the oxidation kettle;

The oxidation kettle also comprises a circulating pump of the heat exchanger and the oxidation kettle, and the circulating port is arranged at the upper part of the other side of the oxidation kettle;

the discharge port of the oxidation kettle is connected with the circulation port through a pipeline, an oxidation kettle circulating pump and a heat exchanger are arranged on the pipeline between the discharge port and the circulation port, the reaction temperature is controlled through the heat exchanger, the material flow c discharged from the discharge port enters the heat exchanger through the oxidation kettle circulating pump, then enters the oxidation kettle through the circulation port, the system pressure is achieved after the reaction time is reached, and the material flow d is discharged from the discharge port of the oxidation kettle.

The discharge port is provided with a regulating valve, and the discharged material flow d is regulated through an oxidation kettle discharge regulating valve of the discharge port.

Set up the stirring leaf in the oxidation kettle, the stirring rate of stirring leaf: 10-500 rpm, make polyethylene wax and hydrogen peroxide distribution more even, promote polyethylene wax oxidation reaction's emergence.

The light component removing kettle comprises a light component removing feed inlet and a light component removing discharge outlet, wherein the light component removing feed inlet is arranged at the middle upper part of one side of the light component removing kettle, and the light component removing discharge outlet is arranged at the lowest discharge liquid level of the light component removing kettle;

the discharge port of the oxidation kettle is connected with the light component removal kettle through a pipeline, a distribution port steam feeding pipe is arranged in the light component removal kettle, the material flow d enters the light component removal kettle, the light component removal kettle releases steam through the distribution port steam feeding pipe, the light component in the polyethylene wax is oxidized by steam stripping, the steam greatly reduces the partial pressure of the light component, the light component in the polyethylene wax is removed, and the material flow g is obtained.

The light component removing kettle further comprises a condensation port, the light component removing feed port is arranged on the upper portion of the other side of the light component removing kettle, a condenser is arranged on a pipeline connected with the condensation port, and the separated material flow e is condensed through the condenser and then is recycled to obtain material flow f, so that secondary utilization can be carried out, the reasonable utilization is realized, and waste is avoided.

The device also comprises a dehydration kettle, wherein the dehydration kettle comprises a dehydration feed inlet, a dehydration discharge outlet and a vacuum port, the dehydration feed inlet is arranged at the middle upper part of one side of the dehydration kettle, the vacuum port is arranged at the upper part of the other side of the dehydration kettle, and the dehydration discharge outlet is arranged at the lowest discharge liquid level of the dehydration kettle;

a discharge port of the lightness removing kettle is connected with a dehydration kettle through a pipeline, a vacuum port is connected with a negative pressure operation mechanism through a pipeline, a material flow g for removing light components enters the dehydration kettle, the vacuum degree of the dehydration kettle is controlled through the negative pressure operation mechanism, after operation is carried out for a period of time, a material flow i of an oxidized polyethylene wax product is obtained, and a discharge pump of the dehydration kettle discharges the material flow to obtain a finished product oxidized polyethylene wax;

the negative pressure operating mechanism is a vacuum pump, and free water separated from the vacuum pump forms a material flow h, so that secondary utilization can be performed, the reasonable utilization is realized, and waste is avoided.

The reaction temperature of the oxidation kettle is 150-180 ℃. The temperature of saturated steam used in the lightness removing kettle is 130-150 ℃, and the operating pressure of the lightness removing kettle is 105-110 KPa. The operation temperature of the dehydration kettle is 120-150 ℃; the operation pressure of the dehydration kettle is 5-50 Kpa.

Example 1

A production device of oxidized polyethylene wax comprises a polyethylene wax storage tank 1, an oxidation kettle 5, a hydrogen peroxide storage tank 3 and a heat exchanger 8;

the oxidation kettle 5-1 comprises a first feeding hole 5-1, a second feeding hole 5-2 and a discharging hole 5-4, wherein the first feeding hole 5-1 and the second feeding hole 5-2 are arranged at the upper part of one side of the oxidation kettle, and the discharging hole 5-4 is arranged at the lowest discharging liquid level of the oxidation kettle;

the polyethylene wax storage tank 1 is connected with a first feeding port 5-1 of the oxidation kettle 5 through a pipeline, and polyethylene wax a in the polyethylene wax storage tank 1 is pumped into the oxidation kettle 5 through a feeding pump 2; the hydrogen peroxide solution storage tank 2 is connected with a second feed inlet 5-2 of the oxidation kettle 5 through a pipeline, and hydrogen peroxide solution b in the hydrogen peroxide solution storage tank 3 is pumped into the oxidation kettle 5 through a feed pump 4; polyethylene wax and hydrogen peroxide are oxidized in an oxidation kettle 5 according to a certain mass ratio under the action of a catalyst to perform oxidation reaction to obtain a material flow c, and the material flow c is discharged through a discharge port 5-4.

Example 2

the polyethylene wax storage tank 1 is connected with a first feeding hole 5-1 of the oxidation kettle 5 through a pipeline, and polyethylene wax in the polyethylene wax storage tank 1 is pumped into the oxidation kettle 5 through a feeding pump 2; the hydrogen peroxide storage tank 2 is connected with a second feed inlet 5-2 of the oxidation kettle 5 through a pipeline, and hydrogen peroxide in the hydrogen peroxide storage tank 3 is pumped into the oxidation kettle 5 through a feed pump 4; polyethylene wax and hydrogen peroxide are oxidized in an oxidation kettle 5 under the action of a catalyst according to a certain mass ratio to carry out oxidation reaction to obtain a material flow c;

the oxidation kettle also comprises a heat exchanger 8 and an oxidation kettle circulating pump 6, and the oxidation kettle also comprises a circulating port which is arranged at the upper part of the other side of the oxidation kettle;

the discharge port 5-4 is connected with the circulation port 5-3 of the oxidation kettle 5 through a pipeline, an oxidation kettle circulating pump 6 and a heat exchanger 8 are arranged on the pipeline between the discharge port 5-4 and the circulation port 5-3, the discharge port 5-4 is provided with an adjusting valve 7, the reaction temperature is controlled through the heat exchanger 8, specifically, a material flow c is discharged from the discharge port of the oxidation kettle 5, the material flow c enters the heat exchanger 8 through the circulating pump to reach the reaction temperature, and after the material flow enters the oxidation kettle 5 through the circulation port to reach the reaction time, the material flow d discharged is adjusted through the system pressure by using the oxidation kettle discharging adjusting valve 7.

Wherein, 5-5 stirring blades are arranged in the oxidation kettle 5, and the stirring speed is as follows: 10-500 rpm, make polyethylene wax and hydrogen peroxide distribution more even, promote polyethylene wax oxidation reaction's emergence.

Example 3

Still include and take off light cauldron 9, take off light cauldron 9 and include and take off light feed inlet, take off light discharge gate, the discharge gate 5-4 of oxidation cauldron 5 passes through pipe connection and takes off light cauldron 9, set up distribution mouth steam inlet pipe 10 in taking off light cauldron 9, oxidation cauldron discharge control valve 7 is adjusted ejection of compact discharge commodity circulation d and is got into and take off light cauldron 9, take off light cauldron 9 and release steam through distribution mouth steam inlet pipe 10, strip the light component in the oxidation low molecular weight polyethylene wax, the light component in the steam will greatly reduced light component partial pressure, the light component in the oxidation low molecular weight polyethylene that the desorption reaction gained obtains, obtain commodity circulation g.

The light component removing process adopts a steam stripping process, so that the partial pressure of light components is greatly reduced, the operation temperature is reduced, and the low odor of the oxidized polyethylene wax is ensured.

The light component removal kettle 9 comprises a condensation port 9-3, and the removed light component and water vapor are condensed by a condenser 11 and then recycled to obtain a material flow f, so that secondary utilization can be carried out, reasonable utilization is realized, and waste is avoided.

Example 4

the discharge port 5-4 is connected with a circulation port 5-3 of the oxidation kettle 5 through a pipeline, an oxidation kettle circulating pump 6 and a heat exchanger 8 are arranged on the pipeline between the discharge port 5-4 and the circulation port 5-3, the discharge port 5-4 is provided with an adjusting valve 7, the reaction temperature is controlled through the heat exchanger 8, specifically, a material flow c is discharged from the discharge port of the oxidation kettle 5, the material flow c enters the heat exchanger 8 through the circulating pump to reach the reaction temperature, and after the material flow c enters the oxidation kettle 5 through the circulation port to reach the reaction time, the material flow d is adjusted through the system pressure by using the oxidation kettle discharge adjusting valve 7.

Still include dehydration cauldron 12 and vacuum pump 13, dehydration cauldron 12 includes dehydration feed inlet 12-1, dehydration discharge gate 12-2 and vacuum port 12-3, 9 discharge gates of lightness-removing cauldron pass through pipeline connection dehydration cauldron 12, the vacuum port passes through pipeline connection vacuum pump 13, the commodity circulation g of desorption light component gets into the dehydration cauldron, vacuum through vacuum pump 13 control dehydration cauldron, operating time is after a period, obtain oxidized polyethylene wax product commodity circulation i, obtain finished product oxidized polyethylene wax by the 14 ejection of compact of dehydration cauldron discharge pump, it forms commodity circulation h to deviate from the free water through vacuum pump 13 simultaneously, can carry out reutilization, rational utilization, avoid extravagant.

The dehydration process adopts vacuum pump negative pressure operation, reduces the operation temperature, thoroughly removes the free water in the oxidized polyethylene wax, and ensures the softening point of the product.

Example 5

the polyethylene wax storage tank 1 is connected with a first feeding port 5-1 of the oxidation kettle 5 through a pipeline, and polyethylene wax in the polyethylene wax storage tank 1 is pumped into the oxidation kettle 5 through a feeding pump 2; the hydrogen peroxide storage tank 2 is connected with a second feed inlet 5-2 of the oxidation kettle 5 through a pipeline, and hydrogen peroxide in the hydrogen peroxide storage tank 3 is pumped into the oxidation kettle 5 through a feed pump 4; polyethylene wax and hydrogen peroxide are oxidized in an oxidation kettle 5 under the action of a catalyst according to a certain mass ratio to carry out oxidation reaction to obtain a material flow c;

Still include and take off light cauldron 9, take off light cauldron 9 including taking off light feed inlet, take off light discharge gate, the discharge gate 5-4 of oxidation cauldron 5 passes through the pipe connection and takes off light cauldron 9, set up distribution mouth steam inlet pipe 10 in taking off light cauldron 9, oxidation cauldron discharge control valve 7 is adjusted ejection of compact discharge commodity circulation d and is got into and take off light cauldron 9, take off light cauldron 9 and pass through distribution mouth steam inlet pipe 10 release steam, strip the light component in the oxidation low molecular weight polyethylene wax, the steam will greatly reduced light component partial pressure, the light component in the oxidation low molecular weight polyethylene that the desorption reaction gained, obtain commodity circulation g.

Polyethylene wax is stored in the polyethylene wax storage tank and is provided with reaction raw materials, hydrogen peroxide is stored in the hydrogen peroxide storage tank and is provided with an oxidant, the oxidation kettle is used as a polyethylene wax and hydrogen peroxide reaction container to produce oxidized polyethylene wax, fire or explosion is not easy to occur, the reaction is mild, the reaction temperature is reduced, the controllability is high, the device safety coefficient is high, light components produced by the product are less, the final product yield is high, the color is good, no pollution is caused, the water content and the ash content are lower, and the acid value of the obtained oxidized polyethylene wax product is moderate.

Application example 1

The method for producing the oxidized polyethylene wax by using the oxidized polyethylene wax production device is characterized in that the polyethylene wax is oxidized by using hydrogen peroxide as an oxidant to prepare the oxidized polyethylene wax;

polyethylene wax is stored in the polyethylene wax storage tank and is provided with reaction raw materials, hydrogen peroxide is stored in the hydrogen peroxide storage tank and is provided with an oxidant, and the oxidation kettle is used as a polyethylene wax and hydrogen peroxide reaction vessel to produce oxidized polyethylene wax, so that fire or explosion is not easy to occur, the reaction is mild, the reaction temperature is reduced, the controllability is high, and the safety coefficient of the device is high.

Application example 2

The method for producing the oxidized polyethylene wax by using the oxidized polyethylene wax production device comprises the following steps:

the method comprises the following steps: hydrogen peroxide is used as an oxidant to carry out oxidation reaction with polyethylene wax; polyethylene wax and hydrogen peroxide are subjected to oxidation reaction under the action of a catalyst according to a certain mass ratio;

Step two: removing light components generated in the synthesis process of the oxidized polyethylene wax;

step three: and removing free water in the oxidized polyethylene wax to obtain the acid oxidized polyethylene wax product.

Application example 3

(1) the polyethylene wax in the polyethylene wax storage tank 1 is pumped into an oxidation kettle 5 through a feed pump 2, the hydrogen peroxide in the hydrogen peroxide storage tank 3 is pumped into the oxidation kettle 5 through a feed pump 4, and the polyethylene wax and the hydrogen peroxide are subjected to oxidation reaction under the action of a catalyst according to a certain mass ratio;

(2) under certain process conditions and under the action of a catalyst, polyethylene wax and hydrogen peroxide are subjected to oxidation reaction in an oxidation kettle 5, the reaction temperature is controlled by a heat exchanger 8, and after the reaction time is up, the discharge is regulated by an oxidation kettle discharge regulating valve 7 through the system pressure, so that a material flow d enters a lightness removing kettle 9;

(3) in a light component removing kettle, removing light components in oxidized polyethylene wax obtained by reaction, releasing steam through a steam feeding pipe 10 at a distribution port, stripping the light components in the oxidized polyethylene wax, greatly reducing the partial pressure of the light components by the steam, and recovering the light components and the steam after condensation by a condenser to obtain a material flow f;

(4) and (3) feeding the material flow g with the light components removed into a dehydration kettle, controlling the vacuum degree of the dehydration kettle by a vacuum pump 13, obtaining a material flow i of the oxidized polyethylene wax product after a period of operation, and discharging the material flow by a discharging pump 14 of the dehydration kettle.

Application example 4

the first step specifically comprises: the first step specifically comprises: (1) the polyethylene wax in the polyethylene wax storage tank 1 is pumped into an oxidation kettle 5 through a feed pump 2, the hydrogen peroxide in the hydrogen peroxide storage tank 3 is pumped into the oxidation kettle 5 through a feed pump 4, and the polyethylene wax and the hydrogen peroxide are subjected to oxidation reaction under the action of a catalyst tetrabutyl titanate according to a certain mass ratio;

the charging conditions are as follows: polyethylene wax stream a: hydrogen peroxide material flow b is 1: 0.09-2 (mass ratio); the concentration of the hydrogen peroxide is 20-30% (mass percentage); the catalyst is tetrabutyl titanate, and the dosage of the tetrabutyl titanate is 0.01-6% of the addition amount of the polyethylene wax;

(2) under certain process conditions and the action of a catalyst, polyethylene wax and hydrogen peroxide are subjected to oxidation reaction in an oxidation kettle 5, the reaction temperature is controlled by a heat exchanger 8, and after the reaction time is up, the discharge is regulated by an oxidation kettle discharge regulating valve 7 through the system pressure, so that a material flow d enters a lightness removing kettle 9;

operating conditions of the oxidation kettle 5: reaction time: 1-5 h, reaction temperature: 150-180 ℃; system pressure: 0.5 to 2MPa (G); stirring speed: 10-500 rpm;

the second step specifically comprises: in a light component removing kettle, removing light components in oxidized polyethylene wax obtained by reaction, releasing steam through a steam feeding pipe 10 at a distribution port, stripping the light components in the oxidized polyethylene wax, greatly reducing the partial pressure of the light components by the steam, condensing the light components and the steam through a condenser, and recovering to obtain a material flow f

The light component removal kettle 9 has the following operating conditions: the saturated steam temperatures used were: the operation time is as follows at 130-150 ℃: 0.5-3 h, operating pressure of 105-110 KPa, steam consumption: oxidized polyethylene wax is 1: 0.2-1.1 (mass ratio);

The third step specifically comprises: and (3) feeding the material flow g without the light components into a dehydration kettle, controlling the vacuum degree of the dehydration kettle by a vacuum pump 13, obtaining a material flow i of the oxidized polyethylene wax product after a period of operation, discharging the material flow i by a discharge pump 14 of the dehydration kettle, wherein the acid value of the finished oxidized polyethylene wax is 18-35 mgKOH/g, and the yield is 92-97%.

Operating conditions of the dehydration kettle 12: the operating temperature is as follows: 120-150 ℃; the operation time is 0.2-2 h, and the operation pressure is 5-50 KPa.

Determining optimal process parameters

Application example 5

In the above-described flow, the operating conditions of the respective operation units are as follows:

(1) the charging conditions are as follows: polyethylene wax stream a: hydrogen peroxide material flow b is 1:0.09 (mass ratio); the concentration of the hydrogen peroxide is 20 percent (mass percentage); the catalyst is tetrabutyl titanate, and the dosage of the tetrabutyl titanate is 0.01 percent of the addition amount of the polyethylene wax.

(2) Operating conditions of the oxidation kettle: reaction time: 1h, reaction temperature: 150 ℃; system pressure: 1.4MPa (G); stirring speed: 200 rpm;

(3) the operating conditions of the light component removal kettle are as follows: the saturated steam temperatures used were: 145 ℃, the operation time is as follows: 3h, operating pressure 105KPa, steam dosage: oxidized polyethylene wax is 1:0.5 (mass ratio);

(4) the operating conditions of the dehydration kettle are as follows: the operating temperature is as follows: 120 ℃; the operating time was 1.0h and the operating pressure was 5 KPa.

Under the process condition, the acid value of the finished oxidized polyethylene wax is 18.6mgKOH/g, and the yield is 92.3 percent.

Application example 6

(3) in a lightness removing kettle, removing light components in oxidized polyethylene wax obtained by reaction, releasing steam through a steam feed pipe 10 at a distribution port, stripping the light components in the oxidized polyethylene wax, greatly reducing the partial pressure of the light components by the steam, and recovering the light components and water vapor after the light components and the water vapor are condensed by a condenser to obtain a material flow f;

In the above-described flow, the operating conditions of the respective operating units are as follows:

(1) the charging conditions are as follows: polyethylene wax stream a: hydrogen peroxide material flow b is 1:0.72 (mass ratio); the concentration of the used hydrogen peroxide is 24.7 percent (mass percentage); the catalyst is tetrabutyl titanate, and the dosage of the tetrabutyl titanate is 1.09 percent of the addition amount of the polyethylene wax.

(2) Operating conditions of the oxidation kettle: reaction time: 2.5h, reaction temperature: 162 ℃; system pressure: 1.6MPa (G); stirring speed: 300 rpm;

(3) the operating conditions of the lightness-removing kettle are as follows: the saturated steam temperatures used were: the operating time is as follows at 150 ℃: 2.1h, operating pressure 108KPa, steam usage: oxidized polyethylene wax is 1:0.8 (mass ratio);

(4) the operating conditions of the dehydration kettle are as follows: the operating temperature is as follows: 135 deg.C; the operation time is 2h and the operation pressure is 10 KPa.

Under the process condition, the acid value of the finished oxidized polyethylene wax is 21.8mgKOH/g, and the yield is 95.1%.

Application example 7

(1) the charging conditions are as follows: polyethylene wax stream a: hydrogen peroxide material flow b is 1:1.1 (mass ratio); the concentration of the hydrogen peroxide is 30 percent (mass percentage); the catalyst is tetrabutyl titanate, and the dosage of the tetrabutyl titanate is 2.41 percent of the addition amount of the polyethylene wax.

(2) Operating conditions of the oxidation kettle: reaction time: 4h, reaction temperature: 170 ℃; system pressure: 1.8MPa (G); stirring speed: 400 rpm;

(3) the operating conditions of the light component removal kettle are as follows: the saturated steam temperatures used were: the operating time is as follows at 150 ℃: 2.5h, operating pressure 110KPa, steam usage: oxidized polyethylene wax is 1:1.1 (mass ratio);

(4) the operating conditions of the dehydration kettle are as follows: the operating temperature is as follows: 150 ℃; the operating time was 2h and the operating pressure was 20 KPa.

Under the process condition, the acid value of the finished oxidized polyethylene wax is 34.4mgKOH/g, and the yield is 96.3 percent

Application example 8

(1) the charging conditions are as follows: polyethylene wax stream a: hydrogen peroxide material flow b is 1:1.2 (mass ratio); the concentration of the hydrogen peroxide is 30 percent (mass percentage); the catalyst is tetrabutyl titanate, and the dosage of the tetrabutyl titanate is 2.41 percent of the addition amount of the polyethylene wax.

(2) Operating conditions of the oxidation kettle: reaction time: 5h, reaction temperature: 180 ℃; system pressure: 1.8MPa (G); stirring speed: 500 rpm;

(4) the operating conditions of the dehydration kettle are as follows: the operating temperature is as follows: 150 ℃; the operation time is 2h, and the operation pressure is 20 KPa.

Under the process condition, the acid value of the finished oxidized polyethylene wax is 35mgKOH/g, and the yield is 97 percent.

Application example 9

(2) under certain process conditions and under the action of a catalyst, polyethylene wax and hydrogen peroxide are subjected to oxidation reaction in an oxidation kettle 5, a reaction temperature heat exchanger 8 is used for controlling, and when the reaction time is up, the discharge is regulated by using an oxidation kettle discharge regulating valve 7 through the system pressure, so that a material flow d enters a lightness removing kettle 9;

(1) the charging conditions are as follows: polyethylene wax stream a: hydrogen peroxide material flow b is 1:0.09 (mass ratio); the concentration of the used hydrogen peroxide is 20 percent (mass percentage); the catalyst is tetrabutyl titanate, and the dosage of the tetrabutyl titanate is 0.01 percent of the addition amount of the polyethylene wax.

(2) Operating conditions of the oxidation kettle 5: reaction time: 1h, reaction temperature: 150 ℃; system pressure: 0.5 (G); stirring speed: 10 rpm;

(3) the light component removal kettle 9 has the following operating conditions: the saturated steam temperatures used were: the operation time is as follows at 130 ℃:0.5 h, operating pressure 105KPa, steam usage: oxidized polyethylene wax is 1:0.2 (mass ratio);

(4) operating conditions of the dehydration kettle 12: the operating temperature is as follows: 120 ℃; the operating time was 0.2 and the operating pressure was 5 KPa.

Under the process condition, the acid value of the finished oxidized polyethylene wax is 18mgKOH/g, and the yield is 92 percent.

Application example 10

(1) the charging conditions are as follows: polyethylene wax stream a: hydrogen peroxide material flow b is 1:2 (mass ratio); the concentration of the hydrogen peroxide is 30 percent (mass percentage); the catalyst is tetrabutyl titanate, and the dosage of the tetrabutyl titanate is 6 percent of the addition amount of the polyethylene wax.

(2) Operating conditions of the oxidation kettle 5: reaction time: 5h, reaction temperature: 180 ℃; system pressure: 2MPa (G); stirring speed: 500 rpm;

(3) the light component removal kettle 9 has the following operating conditions: the saturated steam temperatures used were: the operation time is as follows at 150 ℃: 3h, operating pressure of 110KPa, steam usage: oxidized polyethylene wax is 1:1.1 (mass ratio);

(4) operating conditions of the dehydration kettle 12: the operating temperature is as follows: 150 ℃; the operation time is 0.2-2 h, and the operation pressure is 50 KPa.

Under the process condition, the acid value of the finished oxidized polyethylene wax is 34.2mgKOH/g, and the yield is 96.1 percent.

Finished oxidized polyethylene wax

The acid value and the yield of the finished oxidized polyethylene wax are determined through experiments.

Wherein the acid value is used to indicate the concentration of fatty acid contained in the organic matter, and is the amount of potassium hydroxide consumed in the neutralization of 1g of polyethylene wax with potassium hydroxide. The degree of oxidation can be determined by the acid value, and the higher the acid value, the higher the degree of oxidation.

The yield (actual) amount of the desired product/theoretical amount of the desired product × 100%, (amount of starting material for the desired product/amount of starting material fed × 100%), can be expressed as the actual amount of the desired product as a percentage of the theoretical amount of the desired product calculated for the particular reactant charged.

In conclusion, the acid value and the yield of the finished oxidized polyethylene wax of application example 5 to 10 were determined, and the acid value of the finished oxidized polyethylene wax of application example 8 was 35mgKOH/g, and the yield was 97%. The experimental parameters of example 12 are the optimal parameters, i.e. the optimal process parameters are as follows

(3) the operating conditions of the light component removal kettle are as follows: the saturated steam temperatures used were: the operating time is as follows at 150 ℃: 2.5h, operating pressure of 110KPa, steam dosage: oxidized polyethylene wax is 1:1.1 (mass ratio);

The above embodiments are only examples of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily think of the changes or substitutions within the technical scope of the present invention, and all shall be covered by the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims

1. A production device of oxidized polyethylene wax is characterized by comprising a polyethylene wax storage tank, an oxidation kettle and a hydrogen peroxide storage tank;

2. The apparatus for producing oxidized polyethylene wax according to claim 1, further comprising a heat exchanger and an oxidation kettle circulating pump, wherein the oxidation kettle further comprises a circulating port, and the circulating port is disposed at the upper portion of the other side of the oxidation kettle;

3. The apparatus for producing the oxidized polyethylene wax according to claim 2, wherein the discharge port is provided with a regulating valve, and the discharge stream d is regulated by an oxidizing kettle discharge regulating valve of the discharge port.

4. The apparatus for producing the oxidized polyethylene wax according to claim 1, 2 or 3, wherein a stirring blade is provided in the oxidation vessel, and the stirring speed of the stirring blade is: 10-500 rpm, so that the polyethylene wax and the hydrogen peroxide are distributed more uniformly.

5. The apparatus for producing oxidized polyethylene wax according to claim 3, further comprising a lightness removing kettle, wherein the lightness removing kettle comprises a lightness removing inlet and a lightness removing outlet, the lightness removing inlet is disposed at the middle upper portion of one side of the lightness removing kettle, and the lightness removing outlet is disposed at the lowest discharge level of the lightness removing kettle;

6. The apparatus for producing oxidized polyethylene wax according to claim 5, wherein the lightness removing vessel further comprises a condensation port, the lightness removing feed port is disposed at the upper portion of the other side of the lightness removing vessel, a condenser is disposed on a pipeline connected to the condensation port, and the removed material flow e is condensed by the condenser through the pipeline of the condensation port to obtain a material flow f.

7. The apparatus for producing oxidized polyethylene wax according to claim 6, further comprising a dehydration kettle, wherein the dehydration kettle comprises a dehydration feed inlet, a dehydration discharge outlet, and a vacuum port, the dehydration feed inlet is disposed at the middle upper portion of one side of the dehydration kettle, the vacuum port is disposed at the upper portion of the other side of the dehydration kettle, and the dehydration discharge outlet is disposed at the lowest discharge level of the dehydration kettle;

the discharge port of the light component removal kettle is connected with a dehydration kettle through a pipeline, the vacuum port is connected with a negative pressure operation mechanism through a pipeline, a material flow g for removing light components enters the dehydration kettle, the vacuum degree of the dehydration kettle is controlled through the negative pressure operation mechanism, and a discharge pump of the dehydration kettle discharges the material to obtain a finished product oxidized polyethylene wax;

8. The apparatus for producing oxidized polyethylene wax according to claim 7, wherein the reaction temperature of the oxidation kettle is 150-180 ℃.

9. The apparatus for producing oxidized polyethylene wax according to claim 7, wherein the temperature of the saturated steam used in the lightness removing kettle is 130 to 150 ℃, and the operating pressure of the lightness removing kettle is 105 to 110 KPa.

10. The apparatus for producing oxidized polyethylene wax according to claim 7, wherein the operating temperature of the dehydration kettle is 120-150 ℃; the operation pressure of the dehydration kettle is 5-50 Kpa.