CN110305584B

CN110305584B - PE wax for hot-melt road marking paint and preparation method thereof

Info

Publication number: CN110305584B
Application number: CN201910633866.9A
Authority: CN
Inventors: 李宏伟
Original assignee: Inner Mongolia Zhanyuan Material Technology Co ltd
Current assignee: Inner Mongolia Zhanyuan Material Technology Co ltd
Priority date: 2019-07-15
Filing date: 2019-07-15
Publication date: 2021-02-02
Anticipated expiration: 2039-07-15
Also published as: CN110305584A

Abstract

The invention relates to the technical field of mixed wax, and particularly relates to PE wax for a hot-melt road marking coating and a preparation method thereof. The PE wax is prepared from 95 type refined Fischer-Tropsch wax, zinc stearate, high molecular polyethylene wax and PE oligomer through the operation steps of mixing, heating, stirring and the like. The PE wax disclosed by the invention has the advantages of super-strong dispersing property, adhesive force, proper construction opening time, excellent surface leveling and system anti-settling effects, and good anti-fouling and wetting properties, and is suitable for being used for road marking paint.

Description

PE wax for hot-melt road marking paint and preparation method thereof

Technical Field

The invention relates to the technical field of mixed wax, and particularly relates to PE wax for a hot-melt road marking coating and a preparation method thereof.

Background

The road traffic marking is mainly marked on the road surface and suffers from the impact and abrasion of vehicles due to the sun, rain, wind, snow and freezing, so that the road traffic marking has strict requirements on the performance. Firstly, the drying time is required to be short, and the operation is simple so as to reduce traffic interference; secondly, the reflective power is required to be strong, the color is bright, the reflective power is strong, and the visibility is good in the day and at night; thirdly, it should have skid resistance and wear resistance to ensure driving safety and service life. The road marking is divided into: hot melt marking, normal temperature cold lacquer marking, colored anti-skidding marking, vibration anti-skidding reflection of light marking and preforming marking. The hot-melt marked line is the most widely applied marked line on the road marked line in China. Its advantages are short construction time, high antiwear nature and low cost.

The invention patent application CN 109401516A discloses a production of a road raised marking material, the formula takes petroleum resin, polyethylene wax, titanium pigment, glass beads, plasticizer and stone powder as raw materials, and the preparation method comprises the following steps: weighing petroleum resin, polyethylene wax, titanium dioxide, glass beads, plasticizer and stone powder; putting the materials into grinding equipment for grinding until the materials become fine particles; uniformly feeding the ground fine particles into a stirrer to be uniformly stirred; manually or automatically feeding the uniformly stirred and mixed mixture into a filtering device for filtering; the filtered large particles which are not ground and grinded enter a grinding procedure for reuse; adding the filtered mixed material into an extruder, and performing melt extrusion in a heating state to obtain a marking material; the marking material is packaged by a plastic packaging bag, so that the material has high stability, high light reflection and high stereoscopic impression; the preparation method is simple and clear, has clear steps, and is suitable for popularization and application in the technical field of marking paint. However, the product of the invention has the problems of poor fluidity, poor dispersibility and the like in the using process.

The invention patent application CN 106833349A relates to a polyurethane road marking two-component coating and a preparation method thereof, belonging to the technical field of polyurethane application. The polyurethane road marking bicomponent coating is prepared from the following raw materials in parts by weight: polyether polyol A56-82 parts, polyether polyol B10-20 parts, polyisocyanate 8-40 parts, vulcanizing agent 6-25 parts, catalyst 0.5-1.6 parts, glass beads 5-15 parts and coloring pigment 8-15 parts; the molecular weight of the polyether polyol A is 950-1100, the functionality is 2, and the molecular weight of the polyether polyol B is 2900-3100, and the functionality is 3. The polyurethane road marking bicomponent coating disclosed by the invention is solvent-free, non-toxic, odorless, low in heating temperature, low in viscosity, simple in construction, good in adhesion, strong in ground grabbing force, low in hardness, free of vibration for passing vehicles and wear-resistant; the invention also provides a simple and feasible preparation method. However, the invention has poor anti-pollution and wetting performance and brings much inconvenience when in use.

Through research, the hot-melt road marking paint has the advantages of ultra-strong dispersing performance, adhesive force, proper construction open time, excellent surface leveling and system anti-settling effect, and good anti-fouling and wetting performance. The loss of any one performance can bring adverse effect to the construction quality, thereby affecting the engineering quality, affecting the engineering acceptance time and causing certain economic loss to engineering contractors. This places even greater demands on the PE wax product within the formulation. The PE wax products supplied in the industry in the market are different in quality, almost no PE wax product has the characteristics, so that the PE wax products can be purchased from different raw materials of manufacturers without any unified standard, and the PE wax products are difficult to be selected to the greatest extent.

The invention patent application CN 103756396A discloses a mixed wax for enhancing the smoothness of a coating and a preparation method thereof: adding a certain amount of dispersing agent, initiator and polyethylene wax PE/hexafluoropropylene tripolymer/silyl vinyl unsaturated silane into a reaction kettle, heating to the reaction temperature, and obtaining the polyethylene wax powder grafted on the surface after the reaction is finished. Then mixing with polytetrafluoroethylene PTFE powder, grinding and crushing in a grinding mill to obtain the product of the invention. The surface of the polyethylene wax sphere is modified by hexafluoropropylene trimer and hydrolytic silyl vinyl unsaturated silane, so that the compatibility of the polyethylene wax sphere with polytetrafluoroethylene is improved. Meanwhile, hexafluoropropylene tripolymer and hydrolytic silyl vinyl unsaturated silane are polymerized to form a network structure with branched chains, which is beneficial to improving the binding force with polytetrafluoroethylene micro powder in blending, so that the hexafluoropropylene tripolymer and the hydrolytic silyl vinyl unsaturated silane can be widely used in various types of water-based coatings or alcohol-soluble coatings. In the using process, the product has poor surface leveling and system anti-settling effects, and is not suitable for being applied to road marking paint.

At present, no PE wax for the hot-melt road marking paint has the advantages of super-strong dispersing performance, adhesive force, proper construction opening time, excellent surface leveling and system anti-settling effects, and good anti-fouling and wetting performances.

Disclosure of Invention

In order to solve the problems of poor dispersibility, improper construction opening time, poor surface leveling and system anti-settling effects, poor anti-fouling and wetting properties and the like of the PE wax for the hot-melt road marking paint in the prior art, the invention provides the PE wax for the hot-melt road marking paint.

A hot-melt PE wax for road marking paint is prepared from the following components: 95 type refined Fischer-Tropsch wax, zinc stearate, high molecular polyethylene wax and PE oligomer.

Further, the coating is prepared from the following components in parts by weight: 70-80% of 95 type refined Fischer-Tropsch wax, 5-10% of zinc stearate, 10-20% of high molecular polyethylene wax and 5-20% of PE oligomer.

Further, the molecular weight of the high molecular polyethylene wax is 10000-15000.

Further, the molecular weight of the PE oligomer was 8000-9000.

Further, the weight portion of the high molecular polyethylene wax and the PE oligomer is 0.5-2: 1.

Further, the weight portion of the high molecular polyethylene wax, that is, the PE oligomer is 0.67: 1.

The invention also provides a preparation method of the PE wax for the hot-melt road marking paint, which comprises the following steps: opening the reaction kettle, heating, adding 95 type Fischer-Tropsch wax, stirring, adding zinc stearate, cooling, stirring, adding high-molecular polyethylene wax, heating, stirring, adding PE oligomer, stirring after complete melting, keeping the temperature to obtain liquid PE wax, granulating the liquid PE wax, and screening to obtain the PE wax.

Further, the reaction kettle is opened to raise the temperature to 140-145 ℃.

Further, adding 95 type Fischer-Tropsch wax, stirring at the stirring speed of 10-20r/min, and stopping stirring until the 95 type Fischer-Tropsch wax is melted.

Further, adding zinc stearate, cooling to 135-139 ℃, stirring at 10-20r/min, and stopping stirring until the zinc stearate is melted.

Further, adding the macromolecular polyethylene wax, heating to 140-145 ℃, and stirring at the speed of 10-20r/min until the macromolecular polyethylene wax is melted.

Further, the PE oligomer is put into the reactor and is stirred for 2 to 4 hours under the conditions of 125-135 ℃ and the stirring speed of 10 to 20r/min after the PE oligomer is completely melted.

Further, the liquid PE wax is granulated through a granulation tower, wherein the granulation tower is a stainless steel tower wall, and a granulation nozzle is a stainless steel mesh nozzle.

Further, screening and sieving by a sieve of 80-100 meshes to obtain the PE wax.

Further, the reaction kettle is a stainless steel kettle.

Furthermore, a conveying pipeline is arranged between the reaction kettle and the granulation tower, the conveying pipeline is a stainless steel pipeline, and the conveying pump is a high-temperature-resistant closed liquid pump.

Still further, the delivery conduit temperature is 130 ℃.

Further, the method comprises the following steps: opening a reaction kettle, heating to 140-, and screening to obtain the PE wax.

According to the comprehensive performance requirement of the hot-melt road marking paint on the wax material, the invention provides a single one-stop product by a composite application technology, comprehensively meets various performances (super-strong dispersion performance, adhesive force, proper construction open time, excellent surface leveling and system anti-settling effect, good anti-fouling and wetting performances), is low in price and is available, and the problem of selection of the wax material product bothering manufacturers is thoroughly solved. The invention adopts advanced melting, mixing, dispersing and dust-free atomization equipment, meets the requirement of a downstream dry mixing process, and is safe and environment-friendly.

Compared with the prior art, the invention has the beneficial effects that:

1. according to the invention, the PE wax is creatively prepared by selecting proper components and proportions, and the obtained product has the advantages of super-strong dispersing property, adhesive force, proper construction open time (construction can be carried out without being influenced by temperature and seasons throughout the year), excellent surface leveling and system anti-settling effect, and good anti-fouling and wetting properties.

2. The invention selects a proper component adding sequence, so that the product obtained by the invention has better performance.

3. The production process has the advantages of simplicity, easiness in operation, energy conservation, environmental friendliness and easiness in industrialization.

Detailed Description

The invention will be further described with reference to specific embodiments, the advantages and features of which will become apparent from the description, but which are given by way of illustration only and are not intended to limit the scope of the invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention.

Example 1

Opening the reaction kettle, heating to 140 ℃, adding 70 parts of 95 type refined Fischer-Tropsch wax, stirring at a stirring speed of 10r/min until the 95 type Fischer-Tropsch wax is melted, then adding 5 parts of zinc stearate, cooling, stirring at a stirring speed of 10r/min until the zinc stearate is melted, then adding 10 parts of macromolecular polyethylene wax with the molecular weight of 10000, heating to 140 ℃, and stirring at a stirring speed of 10r/min until the macromolecular polyethylene wax is melted. Adding 15 parts of PE oligomer with the molecular weight of 9000, completely melting, keeping the temperature and stirring for 2 hours at 125 ℃ and at the stirring speed of 10r/min to obtain liquid PE wax, granulating the liquid PE wax through a stainless steel mesh nozzle, and screening and sieving through a 80-mesh sieve to obtain the PE wax.

Example 2

Opening the reaction kettle, heating to 145 ℃, adding 70 parts of 95 type refined Fischer-Tropsch wax, stirring at a stirring speed of 20r/min until the 95 type Fischer-Tropsch wax is melted, then adding 10 parts of zinc stearate, cooling, stirring at a stirring speed of 20r/min until the zinc stearate is melted, then adding 10 parts of macromolecular polyethylene wax with the molecular weight of 10000, heating to 145 ℃, and stirring at a stirring speed of 20r/min until the macromolecular polyethylene wax is melted. Adding 10 parts of PE oligomer with the molecular weight of 8000, completely melting, keeping the temperature and stirring for 4 hours at 135 ℃ and the stirring speed of 20r/min to obtain liquid PE wax, then granulating the liquid PE wax through a stainless steel mesh nozzle, and screening and sieving through a 100-mesh sieve to obtain the PE wax.

Example 3

Opening the reaction kettle, heating to 142 ℃, adding 80 parts of 95 type refined Fischer-Tropsch wax, stirring at a stirring speed of 15r/min until the 95 type Fischer-Tropsch wax is melted, then adding 5 parts of zinc stearate, cooling, stirring at a stirring speed of 18r/min until the zinc stearate is melted, then adding 10 parts of macromolecular polyethylene wax with a molecular weight of 12000, heating to 142 ℃, and stirring at a stirring speed of 12r/min until the macromolecular polyethylene wax is melted. Adding 5 parts of PE oligomer with the molecular weight of 8500, completely melting, stirring at 130 ℃ and the stirring speed of 14r/min for 2h under the condition of heat preservation to obtain liquid PE wax, then granulating the liquid PE wax through a stainless steel mesh nozzle, and screening and sieving through a 90-mesh sieve to obtain the PE wax.

Comparative example 1

Compared with example 1, the addition amount of each component is different.

Opening the reaction kettle, heating to 140 ℃, adding 70 parts of 95 type refined Fischer-Tropsch wax, stirring at a stirring speed of 10r/min until the 95 type Fischer-Tropsch wax is melted, then adding 15 parts of zinc stearate, cooling, stirring at a stirring speed of 10r/min until the zinc stearate is melted, then adding 5 parts of macromolecular polyethylene wax with the molecular weight of 10000, heating to 140 ℃, and stirring at a stirring speed of 10r/min until the macromolecular polyethylene wax is melted. Adding 5 parts of PE oligomer with the molecular weight of 9000, completely melting, keeping the temperature and stirring for 2 hours at 125 ℃ and at the stirring speed of 10r/min to obtain liquid PE wax, granulating the liquid PE wax through a stainless steel mesh nozzle, and screening and sieving through a 80-mesh sieve to obtain the PE wax.

Comparative example 2

Compared with example 1, the weight ratio of the high molecular polyethylene wax to the PE oligomer is 3: 1.

Opening the reaction kettle, heating to 140 ℃, adding 70 parts of 95 type refined Fischer-Tropsch wax, stirring at a stirring speed of 10r/min until the 95 type Fischer-Tropsch wax is melted, then adding 5 parts of zinc stearate, cooling, stirring at a stirring speed of 10r/min until the zinc stearate is melted, then adding 9 parts of macromolecular polyethylene wax with the molecular weight of 10000, heating to 140 ℃, and stirring at a stirring speed of 10r/min until the macromolecular polyethylene wax is melted. Adding 3 parts of PE oligomer with the molecular weight of 9000, completely melting, keeping the temperature and stirring for 2 hours at 125 ℃ and at the stirring speed of 10r/min to obtain liquid PE wax, granulating the liquid PE wax through a stainless steel mesh nozzle, and screening and sieving through a 80-mesh sieve to obtain the PE wax.

Comparative example 3

The order of addition of the components is different compared to example 1.

Opening the reaction kettle, heating to 140 ℃, adding 70 parts of 95 type refined Fischer-Tropsch wax, stirring at a stirring speed of 10r/min until the 95 type Fischer-Tropsch wax is melted, then adding 10 parts of macromolecular polyethylene wax with the molecular weight of 10000, heating to 140 ℃, stirring at a stirring speed of 10r/min until the macromolecular polyethylene wax is melted, then adding 5 parts of zinc stearate, cooling, and stirring at a stirring speed of 10r/min until the zinc stearate is melted. Adding 15 parts of PE oligomer with the molecular weight of 9000, completely melting, keeping the temperature and stirring for 2 hours at 125 ℃ and at the stirring speed of 10r/min to obtain liquid PE wax, granulating the liquid PE wax through a stainless steel mesh nozzle, and screening and sieving through a 80-mesh sieve to obtain the PE wax.

Effect example 1 adhesion

The PE waxes of examples 1 to 3 and comparative examples 1 to 3 were mixed with a varnish and dispersed in the varnish. The test method and the test standard are described in GB-T1720-79, and the results are as follows:

group of	Example 1	Example 2	Example 3	Comparative example 1	Comparative example 2	Comparative example 3
							Adhesion (grade)	7	7	7	5	4	4

Effect example 2 Effect of preventing sedimentation of System

The PE waxes of examples 1 to 3 and comparative examples 1 to 3 were mixed with a varnish, stirred uniformly, and left to stand. The test was accelerated by placing the test at 60 ℃ and observing the time during which no delamination occurred. The test results were as follows:

group of	Example 1	Example 2	Example 3	Comparative example 1	Comparative example 2	Comparative example 3
							Time (moon)	10	9.5	9	7	8	6

Effect example 3 surface leveling Effect

The PE waxes of examples 1 to 3 and comparative examples 1 to 3 were mixed with a varnish, stirred uniformly, and paint samples were applied to a sample with a varnish so as to be smooth and uniform, and then a brush mark was longitudinally smeared in the middle of the coating film with a brush, and it was observed how much time the brush mark disappeared and the coating film returned to a smooth surface. Generally rated in terms of the time for the coating film to reach a uniform smooth surface: good results were obtained in less than 10 minutes; qualified after 10-15 minutes; the test results are as follows, if the sample is not uniform after 15 minutes:

group of	Example 1	Example 2	Example 3	Comparative example 1	Comparative example 2	Comparative example 3
							Time (min)	5	5	7	11	12	15

Effect example 4 antifouling Properties

The PE waxes of examples 1-3 and comparative examples 1-3 were mixed with the clear coat, stirred evenly, and the paint samples were painted onto primed panels and allowed to air dry. The test solvent was dropped onto the panel and covered with a glass cover. After 16 hours, carefully observe whether there was a change in the board surface.

The evaluation criteria are as follows: 0-surface damage evident, severe damage; 1-slight surface breakage; 2-slight expansion, no damage and color change on the surface; 3-slight air bubbles exist on the surface, and the color changes; 4-slight change in color or brightness; 5-No change in surface.

The test results were as follows:

solvent(s)	Example 1	Example 2	Example 3	Comparative example 1	Comparative example 2	Comparative example 3
							Water (W)	5	5	5	4	4	4
Coffee	5	5	5	3	4	3
							Acetic acid	5	5	5	2	3	2

The comprehensive test result shows that the method has the following advantages:

1. according to the invention, the PE wax is creatively prepared by selecting proper components and proportions, and the obtained product has the advantages of super-strong dispersing property, adhesive force, proper construction opening time, excellent surface leveling and system anti-settling effect, and good anti-fouling and wetting properties.

The technical means disclosed by the scheme of the invention are not limited to the technical means disclosed above, and the technical means also comprises the technical scheme formed by any combination of the technical features. While the foregoing is directed to embodiments of the present invention, it will be appreciated by those skilled in the art that various changes and modifications may be made without departing from the principles of the invention, and it is intended to claim all such modifications and alterations as fall within the true scope of the invention.

Claims

1. The PE wax for the hot-melt road marking paint is characterized by being prepared from the following components: the adhesive is prepared from the following components in parts by weight: 70-80 parts of 95 type Fischer-Tropsch wax, 5-10 parts of zinc stearate, 10-20 parts of high molecular polyethylene wax and 5-20 parts of PE oligomer; the molecular weight of the macromolecular polyethylene wax is 10000-15000; the molecular weight of the PE oligomer is 8000-9000;

the preparation method of the PE wax comprises the following steps: opening a reaction kettle, heating, adding 95 type Fischer-Tropsch wax, stirring, adding zinc stearate, cooling, stirring, adding high-molecular polyethylene wax, heating, stirring, adding a PE oligomer, stirring after complete melting, keeping the temperature to obtain liquid PE wax, granulating the liquid PE wax, and screening to obtain the PE wax; the reaction kettle is opened and the temperature is raised to 140-145 ℃.

2. The process for the preparation of PE wax according to claim 1, characterized in that it comprises the following steps: opening a reaction kettle, heating, adding 95 type Fischer-Tropsch wax, stirring, adding zinc stearate, cooling, stirring, adding high-molecular polyethylene wax, heating, stirring, adding a PE oligomer, stirring after complete melting, keeping the temperature to obtain liquid PE wax, granulating the liquid PE wax, and screening to obtain the PE wax; the reaction kettle is opened and the temperature is raised to 140-145 ℃.

3. The preparation method according to claim 2, wherein the type 95 Fischer-Tropsch wax is added and stirred at a stirring speed of 10-20r/min until the type 95 Fischer-Tropsch wax is melted.

4. The method as claimed in claim 2, wherein the temperature of zinc stearate is decreased to 135-139 ℃, the stirring speed is 10-20r/min, and the stirring is stopped until the zinc stearate is melted.

5. The preparation method according to claim 2, wherein the high molecular polyethylene wax is added, the temperature is raised to 140-145 ℃, the stirring speed is 10-20r/min, and the stirring is stopped until the high molecular polyethylene wax is melted; adding PE oligomer, melting completely, stirring at 125-135 deg.C at stirring speed of 10-20r/min for 2-4 h.

6. The method according to claim 2, wherein the PE wax in liquid form is granulated by a granulation tower, wherein the granulation tower is a stainless steel tower wall and the granulation nozzle is a stainless steel mesh nozzle.

7. The method of claim 2, wherein the PE wax is obtained by sieving through a 80-100 mesh sieve.