Low-temperature rapid water-based petroleum resin emulsion and preparation method thereof
By grinding petroleum resin and other raw materials in a sand mill at low temperature, the problems of low preparation efficiency and large energy consumption of existing aqueous petroleum resin emulsions are solved, and an efficient and energy-saving preparation process is achieved.
Patent Information
- Application Number
- CN202510182973.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-19
- Publication Date
- 2025-05-27
AI Technical Summary
The existing preparation methods for aqueous petroleum resin emulsions are inefficient and have high energy consumption, involving high temperature melting and cooling processes.
The low-temperature rapid preparation method is adopted, and the petroleum resin, dispersant, emulsifier and functional additive are ground together by a sand mill at a low temperature of 5-15°C to form a stable aqueous petroleum resin emulsion.
It significantly improves the preparation efficiency and saves energy consumption. The obtained aqueous petroleum resin emulsion has the characteristics of high solids content, simple operation and high production efficiency.
Smart Images

Figure CN120040905A_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the chemical industry field and relates to an aqueous petroleum resin emulsion, specifically a low-temperature and fast-drying aqueous petroleum resin emulsion and a preparation method thereof. Background Art
[0002] Petroleum resin has the advantages of low softening point, good fluidity, good adhesiveness, etc. At the same time, the substance is very brittle at normal or low temperatures and is easy to form powder. Currently, it is widely used in industries such as adhesives, sealants, coatings, and inks, and can effectively improve the wettability of the product with the interface, thereby improving the bonding effect between the product and the interface, and is often used as a tackifier in various products.
[0003] With the gradual improvement of people's environmental protection awareness, the demand for water-based materials is increasing. Petroleum resin has a very wide application in many adhesives, coatings and other related products. Therefore, new requirements are put forward for petroleum resin as a tackifier: preparing solid petroleum resin into an aqueous emulsion and applying it to an aqueous system to further expand the application of petroleum resin.
[0004] Patents for the preparation of waterborne petroleum resin emulsions have been made public. For example, the patent with the application number CN201510239975.4 discloses a petroleum resin emulsion and its preparation method. By weight percentage, the raw materials of the petroleum resin emulsion include the following components: 30 - 35% of petroleum resin; 30 - 35% of water; 30 - 35% of naphthenic oil; 3 - 5% of emulsifier; and an appropriate amount of stabilizer. This invention uses water as the dispersion medium and naphthenic oil as the solvent for the petroleum resin. Through emulsification by the emulsifier, the petroleum resin emulsion is prepared, which has stable performance, features such as fast drying, non-toxic, odorless, and safe, and its preparation method is simple, facilitating production and processing. Another example is that the invention patent with the application number 202011513319.6 discloses a preparation method of a solvent-free waterborne petroleum resin emulsion. This invention provides a preparation method of a solvent-free waterborne petroleum resin emulsion, including the following steps: Weigh petroleum resin and modifier A with an electronic balance, add the petroleum resin to the reaction kettle and heat it for dissolution. When the solid substances in the reaction kettle are completely melted, add modifier A for pretreatment. After the pretreatment is completed, keep the temperature and pressure constant for the hot-melt pretreated modified petroleum resin melt. Take emulsifier B and dissolve it with distilled water, and continuously stir until a transparent liquid is formed, then raise the temperature and pressure. Pump the hot-melt pretreated modified petroleum resin melt and the aqueous solution of emulsifier B into a high-pressure homogenizer for emulsification. The high-pressure homogenizer is discharged at room temperature to obtain a solvent-free waterborne petroleum resin emulsion. The use of the combined emulsification process of modification and high-pressure homogenizer effectively shortens the preparation process of the waterborne petroleum resin emulsion, and the operation is simple and efficient. The above patents all add plasticizer components to the petroleum resin to lower the melting temperature of the petroleum resin, or adopt high-temperature and high-pressure methods to enable the petroleum resin to remain in a resin fluid state during the emulsification process, and then dropwise add water containing emulsifier at the same temperature and stir at high speed to form an emulsion through shear and emulsification. Throughout the preparation process, it involves heating to a high temperature for melting, high-temperature emulsification, and then cooling to room temperature, resulting in slow preparation efficiency and a lot of energy waste.
[0005] Currently, the preparation methods of petroleum resin emulsions all involve heating to a high temperature for melting, high-temperature emulsification, and then cooling to room temperature, resulting in slow preparation efficiency and a lot of heating energy waste. Summary of the Invention
[0006] In view of the above technical problems in the prior art, the present invention provides a low-temperature and rapid waterborne petroleum resin emulsion and its preparation method. The low-temperature and rapid waterborne petroleum resin emulsion and its preparation method are to solve the technical problems of slow preparation efficiency and high energy consumption of waterborne petroleum resin emulsions in the prior art.
[0007] The present invention provides a waterborne petroleum resin emulsion of a low-temperature and rapid waterborne petroleum resin emulsion, which is prepared from the following raw materials in parts by weight:
[0008]
[0009] Further, the petroleum resin is C5 petroleum resin, C9 petroleum resin or modified petroleum resin, and its softening point is 60-150°C. This method has better effects especially on high softening point petroleum resin.
[0010] Further, the modified petroleum resin is one or a mixture of two or more of phenolic modified resin, terpene modified resin, and acid modified resin.
[0011] Further, the dispersant is one or more of sodium lignosulfonate, calcium lignosulfonate, sodium dodecyl sulfonate, and calcium dodecyl sulfonate, and preferably sodium lignosulfonate or calcium lignosulfonate.
[0012] Further, the emulsifier is one or more of Span 20, Span 80, Tween 80, fatty acid glyceride, OP-10, OP-4, and OP-20.
[0013] Further, the present invention uses bentonite and hydroxypropyl cellulose as functional aids. Since both of them have thickening, dispersing and other effects, they can effectively improve the situation of re-agglomeration and adhesion of resin small particles that may occur during the sanding process, and improve the sanding and emulsifying efficiency.
[0014] Further, the particle size of the bentonite is between 1um and 50um.
[0015] Further, the temperature of the distilled water is between 5-15°C.
[0016] The present invention also provides a preparation method of a low-temperature and fast-drying aqueous petroleum resin emulsion, which comprises the following steps:
[0017] 1) Weigh each reaction raw material according to parts by weight;
[0018] 2) Put the petroleum resin, dispersant, emulsifier, bentonite, hydroxypropyl cellulose, and low-temperature distilled water into the sand mill at one time according to the ratio; the temperature of the distilled water is between 5-15°C;
[0019] 3) Add sanding beads, turn on the cooling circulating water and start sanding for 20-60 minutes, and control the temperature of the sanding system at 5-15°C during the sanding process;
[0020] 4) After sanding is completed, filter and discharge to obtain the petroleum resin emulsion.
[0021] Further, the solid content of the obtained petroleum resin emulsion is 50-70%.
[0022] Low-temperature system (low temperature ensures that the petroleum resin is brittle, and high temperature makes the petroleum resin not brittle and not easy to break). At low temperature, the petroleum resin is very brittle (brittle and very easy to be broken into powder). The present invention adopts the method of low-temperature sand grinding, adds functional additives bentonite and hydroxypropyl cellulose, emulsifies the petroleum resin during the sand grinding process, and controls the temperature of the sand grinding system between 5-15 °C by means of external circulating water cooling. Since the petroleum resin has low strength and poor toughness at low temperature and is very brittle, the present invention utilizes the grinding function of sand grinding, and the petroleum resin is easily impacted and broken by the grinding beads during the sand grinding process to form very fine particles. At the same time, sand grinding also has the effect of evenly dispersing the dispersant and emulsifier. Under the comprehensive action of emulsifier, dispersant, bentonite, hydroxypropyl cellulose, etc., the broken small particles of petroleum resin form a stable suspension emulsion system. Bentonite and hydroxypropyl cellulose can effectively improve the situation of re-agglomeration and adhesion of small resin particles that may occur during the sand grinding process, and improve the sand grinding and emulsification efficiency.
[0023] Compared with the existing technology, the technical effect of the present invention is positive and obvious. In order to reduce the time and energy consumed by heating and cooling, combined with the characteristics of the petroleum resin itself, the present invention proposes a preparation method of a low-temperature fast waterborne petroleum resin emulsion, which eliminates the processes of heating the raw materials and cooling the finished product, saving time and energy. The waterborne petroleum resin emulsion prepared by the present invention has the characteristics of simple operation, short preparation period, high production efficiency, and energy saving and consumption reduction. Specific embodiments
[0024] Example 1
[0025] Put 100 kg of C5 petroleum resin, 3 kg of sodium dodecyl sulfonate, 5 kg of composite emulsifier (a mixture of Span 20 and fatty acid glyceride), 2 kg of bentonite with a particle size of 1 μm, 1 kg of hydroxypropyl cellulose, and 111 kg of low-temperature distilled water at 15 °C into a sand mill, add an appropriate amount of sand grinding beads, turn on the cooling circulating water and turn on the sand grinding, sand grind for 20 min, control the temperature of the sand grinding system between 5-15 °C during the sand grinding process, after the sand grinding is completed, filter and discharge to obtain a petroleum resin emulsion, and the solid content of the obtained petroleum resin emulsion is 50%.
[0026] Example 2
[0027] Put 100 kg of C9 petroleum resin, 0.5 kg of sodium lignosulfonate, 1 kg of compound emulsifier (a mixture of Tween 80 and OP-10), 0.5 kg of bentonite with a particle size of 50 μm, 0.5 kg of hydroxypropyl cellulose, and 43.9 kg of low-temperature distilled water at 5 °C into a sand mill. Add an appropriate amount of sanding beads, turn on the cooling circulating water and start sanding for 60 min. During the sanding process, control the temperature of the sanding system at 5 - 15 °C. After sanding is completed, filter and discharge to obtain a petroleum resin emulsion. The solid content of the obtained petroleum resin emulsion is 70%.
[0028] Example 3
[0029] Put 100 kg of C9 petroleum resin, 1 kg of calcium lignosulfonate, 2 kg of compound emulsifier (a mixture of glycerol fatty acid ester and OP-20), 1 kg of bentonite with a particle size of 25 μm, 0.8 kg of hydroxypropyl cellulose, and 69.9 kg of low-temperature distilled water at 10 °C into a sand mill. Add an appropriate amount of sanding beads, turn on the cooling circulating water and start sanding for 35 min. During the sanding process, control the temperature of the sanding system at 5 - 15 °C. After sanding is completed, filter and discharge to obtain a petroleum resin emulsion. The solid content of the obtained petroleum resin emulsion is 60%.
[0030] Example 4
[0031] Put 100 kg of modified petroleum resin, 2 kg of calcium dodecylbenzenesulfonate and 1 kg of sodium lignosulfonate, 3 kg of emulsifier (OP-20), 0.6 kg of bentonite with a particle size of 5 μm, 0.6 kg of hydroxypropyl cellulose, and 57.7 kg of low-temperature distilled water at 6 °C into a sand mill. Add an appropriate amount of sanding beads, turn on the cooling circulating water and start sanding for 45 min. During the sanding process, control the temperature of the sanding system at 5 - 15 °C. After sanding is completed, filter and discharge to obtain a petroleum resin emulsion. The solid content of the obtained petroleum resin emulsion is 65%.
[0032] Example 5
[0033] Put 100 kg of C5 petroleum resin, 3 kg of calcium dodecylbenzenesulfonate, 3 kg of compound emulsifier (a mixture of glycerol fatty acid ester and Span80), 1.5 kg of bentonite with a particle size of 10 μm, 0.8 kg of hydroxypropyl cellulose, and 88.6 kg of low-temperature distilled water at 13 °C into a sand mill. Add an appropriate amount of sanding beads, turn on the cooling circulating water and start sanding for 25 min. During the sanding process, control the temperature of the sanding system at 5 - 15 °C. After sanding is completed, filter and discharge to obtain a petroleum resin emulsion. The solid content of the obtained petroleum resin emulsion is 55%.
[0034] Example 6
[0035] Put 100 kg of C9 petroleum resin, 2 kg of calcium dodecyl sulfonate, 2 kg of compound emulsifier (a mixture of glycerol fatty acid ester and OP-20), 2 kg of bentonite with a particle size of 30 μm, 0.5 kg of hydroxypropyl cellulose, and 65.3 kg of low-temperature distilled water at 8 °C into a sand mill, add an appropriate amount of sanding beads, turn on the cooling circulating water and start sanding for 30 min. During the sanding process, control the temperature of the sanding system at 5 - 15 °C. After sanding is completed, filter and discharge to obtain a petroleum resin emulsion. The solid content of the obtained petroleum resin emulsion is 62%.
[0036] Comparative Example 1
[0037] Put 10 kg of liquid paraffin and 90 kg of C5 petroleum resin into a reaction kettle at 160 °C, slowly stir until melted and mixed evenly, which takes about 90 min. Lower the temperature to 120 °C, which takes about 30 min, add 2 kg of sodium dodecyl sulfonate, and stir and mix evenly at 200 rpm, which takes about 20 min; lower the temperature to 95 °C, which takes about 15 min, then dropwise add 50 kg of 18 wt.% compound emulsifier aqueous solution (an aqueous solution mixture of Span 20 and glycerol fatty acid ester), increase the stirring rate to 500 rpm, and stir for 30 min; continue to dropwise add 39 kg of distilled water at the same temperature for dilution, stir at 600 rpm for 30 min, cool down and filter to obtain a petroleum resin emulsion. The solid content of this emulsion is 55.8%. The total time for temperature rise, temperature drop and stirring is about 185 min.
[0038] Comparative Example 2
[0039] Put 10 kg of liquid naphthenic oil and 90 kg of C5 petroleum resin into a reaction kettle at 160 °C, slowly stir until melted and mixed evenly, which takes about 60 min. Lower the temperature to 120 °C, which takes about 30 min, add 2 kg of sodium dodecyl sulfonate, and stir and mix evenly at 200 rpm, which takes about 20 min; lower the temperature to 95 °C, which takes about 15 min, then dropwise add 50 kg of 18 wt.% compound emulsifier aqueous solution (an aqueous solution mixture of Span 20 and glycerol fatty acid ester), increase the stirring rate to 500 rpm, and stir for 30 min; continue to dropwise add 39 kg of distilled water at the same temperature for dilution, stir at 600 rpm for 30 min, cool down and filter to obtain a petroleum resin emulsion. The solid content of this emulsion is 55.8%, and the total time for temperature rise, temperature drop and stirring is about 155 min.
[0040] From the preparation process of the comparative examples, the preparation process of heating and melting, high-temperature emulsification, and cooling and temperature reduction involves heating and cooling in the middle, and the time consumption is relatively long. Through the preparation time, the advantages of the present invention in improving production efficiency can be clearly seen.
Claims
1. A low-temperature, fast-acting aqueous petroleum resin emulsion, characterized in that: It is prepared from the following raw materials in parts by weight:
2. The aqueous petroleum resin emulsion of a low-temperature fast aqueous petroleum resin emulsion according to claim 1, characterized in that: The petroleum resin is C5 petroleum resin, C9 petroleum resin or modified petroleum resin, and its softening point is 60-150°C.
3. The aqueous petroleum resin emulsion of a low-temperature fast aqueous petroleum resin emulsion according to claim 1, characterized in that: The modified petroleum resin is one or a mixture of two or more of phenol modified resin, terpene modified resin and acid modified resin.
4. The aqueous petroleum resin emulsion of a low-temperature fast aqueous petroleum resin emulsion according to claim 1, characterized in that: The dispersant is one or more of sodium lignin sulfonate, calcium lignin sulfonate, sodium dodecyl sulfonate and calcium dodecyl sulfonate.
5. The aqueous petroleum resin emulsion of a low-temperature fast aqueous petroleum resin emulsion according to claim 1, characterized in that: The emulsifier is one or more of Span 20, Span 80, Tween 80, fatty acid glyceride, OP-10, OP-4, and OP-20.
6. The aqueous petroleum resin emulsion of a low-temperature fast aqueous petroleum resin emulsion according to claim 1, characterized in that: The particle size of the bentonite is between 1um and 50um.
7. The aqueous petroleum resin emulsion of a low-temperature fast aqueous petroleum resin emulsion according to claim 1, characterized in that: The temperature of the distilled water is between 5-15°C.
8. The method for preparing a low-temperature fast-acting aqueous petroleum resin emulsion according to claim 1, characterized in that The following steps are involved: 1) Weigh each reaction raw material according to weight; 2) Put petroleum resin, dispersant, emulsifier, bentonite, hydroxypropyl cellulose and distilled water into a sand mill at one time according to the proportion; the temperature of the distilled water is between 5-15°C; 3) Add sanding beads, start the cooling circulating water and start sanding, sanding for 20-60 minutes, and control the temperature of the sanding system at 5-15°C during the sanding process; 4) After sand grinding, the material is filtered to obtain a petroleum resin emulsion.
9. The method for preparing a low-temperature fast-acting aqueous petroleum resin emulsion according to claim 8, characterized in that: The solid content of the obtained petroleum resin emulsion is 50-70%.
Citation Information
Patent Citations
Petroleum resin emulsion and preparation method thereof
CN104845034A
Preparation method of solvent-free water-based petroleum resin emulsion
CN112646201A