Preparation method of environmentally friendly rosin ester emulsion

Abstract

The invention discloses a method for preparing an environmentally friendly rosin ester emulsion, comprising: mixing cardanol polyoxyethylene ether phosphate, alkyl glucoside APG1214, sodium lauroylbenzene sulfonate, and deionized water to obtain a composite bio-based emulsifier aqueous solution; adding a small amount of biomass oil to rosin ester, mixing and heating to melt, adding the emulsifier aqueous solution to the molten rosin ester and mixing evenly; then adding deionized water, emulsifying, adding deionized water to adjust the solid content after phase inversion, cooling, filtering to obtain a rosin ester emulsion with an average particle size of 0.3 μm to 0.4 μm, and D90 less than 0.5 μm. The raw materials of the rosin ester emulsion of the present invention are all bio-based materials, with good biodegradability, and the emulsifier can be compounded at room temperature, which is environmentally friendly and efficient; after adding biomass oil, the melting temperature and emulsification temperature of the rosin ester can be effectively reduced, and production energy consumption can be reduced.

Description

Technical Field

[0001] The invention relates to the technical field of chemical industry, and more specifically to a method for preparing an environmentally friendly rosin ester emulsion. Background Art

[0002] Rosin ester is a green fine chemical product generated by the esterification reaction of polyols and natural rosin. It is an oil-soluble resin and is used as a tackifier in industrial fields such as adhesives and coatings. Rosin ester emulsion can be prepared by studying the emulsification of rosin ester with emulsifiers. Rosin ester emulsion can significantly improve the performance of emulsion adhesives and coatings, and can reduce the cost of adhesives and coatings. Many experts and scholars at home and abroad have studied the preparation method of rosin ester emulsion. After years of development, the preparation process of rosin ester emulsion has become relatively mature. However, in recent years, the price of chemical raw materials has fluctuated greatly, and emulsifiers account for 5-20% of rosin ester emulsions. The cost of traditional emulsifiers has been greatly affected, and the risk of product production and operation has continued to increase. In order to seek sustainable development, bio-based emulsifiers have replaced traditional emulsifiers as an alternative and have received more and more attention. Affected by the global climate environment and facing the increasing pressure on environmental protection, many companies are looking for environmentally friendly, energy-saving and carbon emission-reducing preparation methods to enhance the competitiveness of their products. For example, the Chinese patent with announcement number CN105944621B uses cardanol, polyether modified trisiloxane, ethanol, sodium dodecyl sulfate, etc. as raw materials to prepare a bio-based emulsifier. The rosin emulsion prepared by the emulsifier has the characteristics of good stability and long storage period, but other performances are not reflected, and the improvement performance of pressure-sensitive adhesive is unknown. For example, the Chinese patent with announcement number CN100398619C uses rosin-based polyether carboxylate and palmitic acid agent glucoside as an emulsifier, emulsifies rosin ester under high-speed stirring conditions of 3000-5000rpm, and obtains a rosin ester emulsion with an average particle size of less than 150nm. However, this method uses too high a speed, has high requirements on equipment, and is difficult to promote in the process of large-scale production.

[0003] Therefore, it is a problem that needs to be solved at present to develop a rosin ester emulsion that uses a bio-based emulsifier for emulsification, has a simple process, is environmentally friendly and energy-saving, and can significantly improve the performance of the pressure-sensitive adhesive emulsion. Summary of the invention

[0004] In order to solve the technical deficiencies of the existing rosin ester emulsion, the purpose of the present invention is to provide an environmentally friendly rosin ester emulsion preparation method using a bio-based emulsifier, which has a simple emulsification process and can significantly improve the performance of the pressure-sensitive adhesive emulsion, so as to solve the above problems.

[0005] In order to achieve the purposes of the present invention, the present invention provides a method for preparing an environmentally friendly rosin ester emulsion, comprising:

[0006] Cardanol polyoxyethylene ether phosphate, alkyl glucoside APG1214, sodium lauroylbenzene sulfonate and deionized water are uniformly mixed at room temperature to prepare an emulsifier aqueous solution; rosin ester and biomass oil are mixed together, heated and melted, and the emulsifier aqueous solution is added and mixed uniformly; deionized water is then added for emulsification, and after phase inversion occurs, deionized water is continuously added to adjust the solid content, the temperature is lowered, and the rosin ester emulsion is obtained by filtering.

[0007] Preferably, in the preparation method of the environmentally friendly rosin ester emulsion, the rosin ester is 250 parts, biomass oil is 1-70 parts, cardanol polyoxyethylene ether phosphate is 10-30 parts, alkyl glucoside APG1214 is 3-15 parts, sodium lauroylbenzene sulfonate is 1-10 parts, and some deionized water is used.

[0008] Preferably, in the method for preparing the environmentally friendly rosin ester emulsion, the weight portion of the biomass oil is 5 to 50 parts.

[0009] Preferably, in the method for preparing the environmentally friendly rosin ester emulsion, the weight parts of biomass oil are 12.5 parts, 25 parts or 50 parts.

[0010] Preferably, in the method for preparing the environmentally friendly rosin ester emulsion, the biomass oil is a biomass oil with a solidification point ≤10°C and a decomposition temperature ≥200°C.

[0011] Preferably, in the method for preparing the environmentally friendly rosin ester emulsion, the temperature at which the rosin ester and the biomass oil are mixed and heated is 120°C to 180°C.

[0012] Preferably, in the method for preparing the environmentally friendly rosin ester emulsion, the molten rosin ester is stirred until transparent, and the emulsifier aqueous solution is heated to 60-90°C before being added and mixed; and the temperature of the deionized water is 85-95°C.

[0013] Application of the rosin ester emulsion prepared by the preparation method in the preparation of pressure-sensitive adhesive emulsion.

[0014] The rosin ester emulsion prepared by the preparation method is used in the preparation of acrylic ester pressure-sensitive adhesive emulsion.

[0015] The present invention has at least the following beneficial effects:

[0016] 1. The present invention adopts a new type of green and environmentally friendly composite emulsifier mixed with cardanol polyoxyethylene ether phosphate, alkyl glucoside APG1214, sodium lauroylphenyl sulfonate, and deionized water. All of them are bio-based materials, which reduce the dependence on chemical raw materials, have good biodegradability, can be compounded at room temperature, and have the characteristics of high efficiency and environmental protection.

[0017] 2. The present invention adopts biomass oil as a bio-based plasticizer and flux, which effectively reduces the temperature and time required for resin melting, reduces melt viscosity, improves emulsification efficiency, and reduces stirring speed requirements, reduces equipment requirements, and reduces production energy consumption; in addition, since the molecular weight distribution width of the matrix resin is increased, without sacrificing the tackifying properties of the tackifying resin emulsion for the water-based pressure-sensitive adhesive, the bonding performance of the water-based pressure-sensitive adhesive under low temperature conditions is unexpectedly increased, and the low-temperature initial tack and peel strength are both improved.

[0018] 3. The present invention adopts a compound bio-based emulsifier, which is made of renewable natural raw materials such as cardanol polyoxyethylene ether phosphate, alkyl glycoside emulsifier APG1214, sodium lauroylphenyl sulfonate, etc., and has good biodegradability.

[0019] 4. The raw materials used in the present invention are all renewable bio-based materials, with renewable materials accounting for nearly 100% and having good biodegradability.

[0020] 5. The rosin ester emulsions prepared in Examples 5 to 7 of the present invention have an average particle size of less than 500 nm (0.5 μm), good stability, and can be stored for a long time. At the same time, since the particle size of the emulsion is similar to that of the polymer emulsion, it has good compatibility and is an ideal emulsion tackifier for water-based adhesives.

[0021] Other advantages, objectives and features of the present invention will be embodied in part through the following description, and in part will be understood by those skilled in the art through study and practice of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 is the particle size distribution diagram of the rosin ester emulsion ER1 of Example 1;

[0023] Figure 2 This is the particle size distribution diagram of the rosin ester emulsion ER2 of Example 2;

[0024] Figure 3 This is the particle size distribution diagram of the rosin ester emulsion ER3 of Example 3;

[0025] Figure 4 is the particle size distribution diagram of the rosin ester emulsion ER4 of Example 4;

[0026] Figure 5 is the particle size distribution diagram of the rosin ester emulsion ER5 of Example 5;

[0027] Figure 6 is the particle size distribution diagram of the rosin ester emulsion ER6 of Example 6;

[0028] Figure 7 is the particle size distribution diagram of the rosin ester emulsion ER7 of Example 7;

[0029] Figure 8This is the particle size distribution diagram of the rosin ester emulsion ER8 of Example 8. DETAILED DESCRIPTION

[0030] The present invention is further described in detail below with reference to the accompanying drawings and examples so that those skilled in the art can implement the invention according to the description.

[0031] It should be understood that the terms such as “having”, “including” and “comprising” used herein do not exclude the existence or addition of one or more other elements or combinations thereof.

[0032] It should be noted that the experimental methods described in the following embodiments are conventional methods unless otherwise specified, and the reagents and materials can be obtained from commercial sources unless otherwise specified. The normal temperature is 20-25°C.

[0033] The cardanol polyoxyethylene ether phosphate involved in the examples of the present invention has the characteristics of wide sources, renewability, low toxicity, easy biodegradability, excellent emulsification performance, etc. The present invention uses the cardanol polyoxyethylene ether phosphate as the main emulsifier in the compound emulsifier.

[0034] The alkyl glycoside emulsifier APG1214 involved in the implementation steps of the present invention is specifically composed of a mixture of C12-C14 alkyl glucosides, which has excellent emulsifying properties, high safety, non-toxicity, no irritation, and rapid and thorough biodegradation. Experimental studies have found that in the preparation process of rosin ester emulsion, excessive addition will result in a significant thickening effect, so we choose to add a proportion of no more than 50% of the mass of the main emulsifier. The preferred mass ratio of the alkyl glycoside emulsifier to the cardanol polyoxyethylene ether phosphate is (3-15):20.

[0035] The sodium lauroylbenzene sulfonate involved in the implementation steps of the present invention, also known as sodium dodecylbenzene sulfonate, has excellent emulsification properties and very good biodegradability. However, due to its excellent foaming properties, a large amount of foam is easily generated during the actual emulsification process, so its added content should be controlled. The preferred mass ratio of the sodium lauroylbenzene sulfonate to the cardanol polyoxyethylene ether phosphate is (1-5):20.

[0036] The biomass oil involved in the implementation steps of the present invention can be babassu seed oil, sardine oil, linseed oil, tung oil, walnut oil, soybean oil, safflower oil, sunflower oil, sesame oil, cottonseed oil, corn oil, rapeseed oil, peanut oil, krambey oil, castor oil, olive oil, rapeseed oil, grape seed oil and sesame oil, preferably cottonseed oil, sardine oil, linseed oil, tung oil, walnut oil, soybean oil, safflower oil and sunflower oil, including but not limited to the biomass oils and their mixtures marked above, or the biomass oils and their mixtures with a freezing point of ≤10°C and a decomposition temperature of ≥200°C after secondary use and resource recycling. If the freezing point is too high, it will affect its fluidity and it is difficult to add materials to penetrate into the gaps between the rosin glycerol ester particles. It is preferred that the freezing point is less than 10°C, that is, the biomass oil is in a liquid flow state at room temperature. At the same time, in order to ensure the stability of oil quality, that is, during the emulsification production process, the molecular structure of vegetable oil will not be cracked due to high temperature to produce small molecules that are not conducive to product quality, so biomass oil with a decomposition temperature greater than 200°C is preferred.

[0037] The fatty acids in biomass oils and fats are mainly present in the form of glycerides, which have good compatibility with rosin glycerides. At the same time, the chemical structure of biomass oils and fats contains long and soft fat chains, which makes it have a lower glass transition temperature. When melted and mixed with rosin glycerides in a certain proportion, the overall glass transition temperature Tg of rosin glycerides can be reduced. In addition, because biomass oils and fats have a lower specific heat capacity than rosin glycerides, they heat up faster. Biomass oils and fats are fluid at room temperature and dispersed between rosin particles. Under heating conditions, heat can be transferred to rosin glyceride particles with lower temperatures more quickly, making them heat up faster and evenly, reducing the situation of material accumulation, slow heat transfer efficiency, and partial rosin particles being undercooked. At the same time, it also reduces the temperature and time required for the reactor to heat up, reducing energy consumption.

[0038] The applicant has found that when the biomass oil content exceeds 20% of the mass of rosin glycerol ester, the biomass oil plays a thickening role in the emulsion and increases the viscosity of the emulsion, so its added content cannot exceed 20% of the mass of rosin glycerol ester. When the biomass oil content is less than 2%, the biomass oil added to the rosin glycerol ester will not have a significant performance improvement effect. When the biomass oil content is 2-20% of the mass of rosin glycerol ester, the temperature and time required for the melting of rosin glycerol ester can be reduced, thereby reducing energy consumption and playing the role of a flux.

[0039] The addition of biomass oil improves the resin composition structure of the base resin and improves the low-temperature performance of the base resin. Adding it into the acrylic pressure-sensitive adhesive latex can effectively improve the low-temperature initial adhesion and peel strength of the adhesive, effectively improve its adhesive performance, and play the role of an environmentally friendly plasticizer.

[0040] The rosin ester emulsion preparation method of the invention has good emulsifying effect not only on rosin glycerol ester, but also on rosin pentaerythritol ester and rosin ester with a softening point lower than 120°C and its derivatives.

[0041] The rosin ester emulsion of the invention can be miscible with acrylic resin emulsion, ethylene vinyl acetate emulsion, vinyl acetate copolymer, natural rubber emulsion, styrene-butadiene rubber emulsion, nitrile rubber emulsion, chloroprene rubber emulsion and the like, and can be compounded at room temperature to obtain corresponding emulsion products.

[0042] The formula comparison table for each example below is as follows:

[0043] Table 1 Example formula comparison table

[0044]

[0045] Example 1 Preparation of rosin ester emulsion ER1

[0046] 250 parts of rosin glycerol ester (softening point 90±5℃) are added to a kettle reaction vessel equipped with an anchor stirrer, nitrogen protection, reflux condenser, liquid feed pump, and temperature sensor, and the temperature is raised to 180℃ to melt. The rosin glycerol ester is heated to become a low-viscosity flowing liquid, and the stirring speed is 200rpm, and the resin liquid is stirred until it is transparent. 10 parts of cardanol polyoxyethylene ether phosphate, 15 parts of alkyl glucoside APG1214, and 10 parts of sodium lauroylbenzene sulfonate are dissolved in 100 parts of deionized water, stirred evenly at room temperature, and heated to 60-90℃ to obtain a composite emulsifier aqueous solution. The feed pump adds the emulsifier aqueous solution into the reactor at 5ml / min. After the addition of the emulsifier aqueous solution, deionized water at 85-95° C. was added at 5 ml / min through a feed pump, and the stirring speed was increased to 300 rpm. When phase inversion occurred, the speed was reduced to 80 rpm, and deionized water was continued to be added to adjust the solid content to 50%. The temperature was lowered to below 40° C. and filtered through a 100-mesh stainless steel filter to obtain rosin ester emulsion ER1 with a solid content of about 50%, an average particle size of less than 1.7 μm, and a viscosity of less than 200 mPa.s. Under an environment of 5-40° C., precipitation occurred on the second day.

[0047] Example 2 Preparation of rosin ester emulsion ER2

[0048] 250 parts of rosin glycerol ester (softening point 90±5°C) are added into a kettle reaction vessel equipped with an anchor stirrer, nitrogen protection, reflux condenser, liquid feeding pump, and temperature sensor, and the temperature is raised to 180°C for melting. The rosin glycerol ester is heated to become a low-viscosity flowing liquid. The stirring speed is 200rpm, and the resin liquid is stirred until it is transparent. 30 parts of cardanol polyoxyethylene ether phosphate, 3 parts of alkyl glucoside APG1214, and 1 part of sodium lauroylbenzene sulfonate are dissolved in 100 parts of deionized water, stirred evenly at room temperature, and heated to 60-90°C to obtain a composite emulsifier aqueous solution. The feeding pump adds the emulsifier aqueous solution into the reactor at 5ml / min. After the emulsifier aqueous solution is added, deionized water at 85-95° C. is added at 5 ml / min through a feed pump, and the stirring speed is increased to 300 rpm. When phase inversion occurs, the speed is reduced to 80 rpm, and deionized water is continued to be added to adjust the solid content to 50%. The temperature is lowered to below 40° C. and filtered through a 100-mesh stainless steel filter to obtain rosin ester emulsion ER2 with a solid content of about 50%, an average particle size of less than 0.9 μm, and a viscosity of less than 200 mPa.s. The storage period is greater than 60 days at 5-40° C.

[0049] Example 3 Preparation of rosin ester emulsion ER3

[0050] 250 parts of rosin glycerol ester (softening point 90±5°C) are added into a kettle reaction vessel equipped with an anchor stirrer, nitrogen protection, reflux condenser, liquid feeding pump, and temperature sensor, and the temperature is raised to 180°C for melting. The rosin glycerol ester is heated to become a low-viscosity flowing liquid. The stirring speed is 200rpm, and the resin liquid is stirred until it becomes transparent. 18 parts of cardanol polyoxyethylene ether phosphate, 5 parts of alkyl glucoside APG1214, and 3 parts of sodium lauroylbenzene sulfonate are dissolved in 100 parts of deionized water, stirred evenly at room temperature, and heated to 60-90°C to obtain an emulsifier aqueous solution. The feeding pump adds the emulsifier aqueous solution into the reactor at 5ml / min. After the addition of the emulsifier aqueous solution, 85-95°C deionized water was added at 5 ml / min through a feed pump, and the stirring speed was increased to 300 rpm. When phase inversion occurred, the speed was reduced to 80 rpm, and deionized water was continued to be added to adjust the solid content to 50%. The temperature was lowered to below 40°C, and the mixture was filtered through a 100-mesh stainless steel filter to obtain rosin ester emulsion ER3, which had a solid content of about 50%, an average particle size of <0.6 μm, a viscosity of <200 mpa.s, and a storage period of >180 days at 5-40°C. Example 4 Preparation of rosin glycerol ester (+2% vegetable oil) emulsion ER4

[0051] 250 parts of rosin glycerol ester (softening point 90±5°C) and 5 parts of cottonseed oil are added into a kettle reaction vessel equipped with an anchor stirrer, nitrogen protection, reflux condenser, liquid feeding pump, and temperature sensor, and the temperature is raised to 150°C for melting. The rosin glycerol ester is heated to become a low-viscosity flowing liquid. The stirring speed is 200 rpm and the resin liquid is stirred until it becomes transparent. 18 parts of cardanol polyoxyethylene ether phosphate, 5 parts of alkyl glucoside APG1214, and 3 parts of sodium lauroylbenzene sulfonate are dissolved in 100 parts of deionized water, stirred evenly at room temperature, and heated to 60-90°C to obtain an emulsifier aqueous solution. The feeding pump adds the emulsifier aqueous solution into the reactor at 5 ml / min. After the addition of the emulsifier aqueous solution, 85-95°C deionized water was added at 5 ml / min through a feed pump, and the stirring speed was increased to 300 rpm. When the phase inversion occurred, the speed was reduced to 80 rpm, and deionized water was continued to be added to adjust the solid content to 50%. The temperature was lowered to below 40°C, and the mixture was filtered through a 100-mesh stainless steel filter to obtain rosin ester emulsion ER4, which had a solid content of about 50%, an average particle size of less than 0.6 μm, and a viscosity of less than 200 mPa.s. Under an environment of 5-40°C, the storage period was greater than 180 days. Example 5 Preparation of rosin glycerol ester (+5% vegetable oil) emulsion ER5

[0052] 250 parts of rosin glycerol ester (softening point 90±5°C) and 12.5 parts of cottonseed oil are added into a kettle reaction vessel equipped with an anchor stirrer, nitrogen protection, reflux condenser, liquid feeding pump and temperature sensor, and the temperature is raised to 120-150°C for melting. The rosin glycerol ester is heated to become a low-viscosity flowing liquid, and the stirring speed is 200 rpm, and the resin liquid is stirred until it becomes transparent; 18 parts of cardanol polyoxyethylene ether phosphate, 5 parts of alkyl glucoside APG1214, and 3 parts of sodium lauroylbenzene sulfonate are dissolved in 100 parts of deionized water, stirred evenly at room temperature, and heated to 60-90°C to obtain an emulsifier aqueous solution, and the feeding pump adds the emulsifier aqueous solution into the reactor at 5 ml / min. After the emulsifier aqueous solution is added, deionized water at 85-95° C. is added at 5 ml / min through a feed pump, and the stirring speed is increased to 300 rpm. When phase inversion occurs, the speed is reduced to 80 rpm, and deionized water is continued to be added to adjust the solid content to 50%. The temperature is lowered to below 40° C. and filtered through a 100-mesh stainless steel filter to obtain rosin ester emulsion ER5 with a solid content of about 50%, an average particle size of less than 0.4 μm, and a viscosity of less than 200 mPa.s. The storage period is greater than 180 days at 5-40° C.

[0053] Example 6 Preparation of rosin glycerol ester (+10% vegetable oil) emulsion ER6

[0054] 250 parts of rosin glycerol ester (softening point 90±5°C) and 25 parts of cottonseed oil are added into a kettle reaction vessel equipped with an anchor stirrer, nitrogen protection, reflux condenser, liquid feeding pump and temperature sensor, and the temperature is raised to 120-150°C for melting. The rosin glycerol ester is heated to become a low-viscosity flowing liquid, and the stirring speed is 200 rpm, and the resin liquid is stirred until it becomes transparent; 18 parts of cardanol polyoxyethylene ether phosphate, 5 parts of alkyl glucoside APG1214, and 3 parts of sodium lauroylbenzene sulfonate are dissolved in 100 parts of deionized water, stirred evenly at room temperature, and heated to 60-90°C to obtain an emulsifier aqueous solution. The feeding pump adds the emulsifier aqueous solution into the reactor at 5 ml / min. After the addition of the emulsifier aqueous solution, deionized water at 85-95°C was added at 5 ml / min through a feed pump, and the stirring speed was increased to 300 rpm. When phase inversion occurred, the speed was reduced to 80 rpm, and deionized water was continued to be added to adjust the solid content to 50%. The temperature was lowered to below 40°C, and the mixture was filtered through a 100-mesh stainless steel filter to obtain rosin ester emulsion ER6, which had a solid content of about 50%, an average particle size of less than 0.4 μm, and a viscosity of less than 200 mPa.s. Under an environment of 5-40°C, the storage period was greater than 180 days. Example 7 Preparation of rosin glycerol ester (+20% vegetable oil) emulsion ER7

[0055] 250 parts of rosin glycerol ester (softening point 90±5°C) and 50 parts of cottonseed oil are added into a kettle reaction vessel equipped with an anchor stirrer, nitrogen protection, reflux condenser, liquid feeding pump and temperature sensor, and the temperature is raised to 120-150°C for melting. The rosin glycerol ester is heated to become a low-viscosity flowing liquid, and the stirring speed is 200 rpm, and the resin liquid is stirred until it is transparent; 18 parts of cardanol polyoxyethylene ether phosphate, 5 parts of alkyl glucoside APG1214, and 3 parts of sodium lauroylbenzene sulfonate are dissolved in 100 parts of deionized water, stirred evenly at room temperature, and heated to 60-90°C to obtain an emulsifier aqueous solution. The feeding pump adds the emulsifier aqueous solution into the reactor at 5 ml / min. After the emulsifier aqueous solution is added, deionized water at 85-95° C. is added at 5 ml / min through a feed pump, and the stirring speed is increased to 300 rpm. When phase inversion occurs, the speed is reduced to 80 rpm, and deionized water is continued to be added to adjust the solid content to 50%. The temperature is lowered to below 40° C. and filtered through a 100-mesh stainless steel filter to obtain rosin ester emulsion ER7 with a solid content of about 50%, an average particle size of less than 0.4 μm, and a viscosity of less than 200 mPa.s. The storage period is greater than 180 days at 5-40° C.

[0056] Example 8 Preparation of Rosin Glycerol Ester (+25% Vegetable Oil) Emulsion ER8

[0057] 250 parts of rosin glycerol ester (softening point 90±5°C) and 62.5 parts of cottonseed oil are added into a kettle reaction vessel equipped with an anchor stirrer, nitrogen protection, reflux condenser, liquid feeding pump and temperature sensor, and the temperature is raised to 120-150°C for melting. The rosin glycerol ester is heated to become a low-viscosity flowing liquid, and the stirring speed is 200 rpm, and the resin liquid is stirred until it becomes transparent; 18 parts of cardanol polyoxyethylene ether phosphate, 5 parts of alkyl glucoside APG1214, and 3 parts of sodium lauroylbenzene sulfonate are dissolved in 100 parts of deionized water, stirred evenly at room temperature, and heated to 60-90°C to obtain an emulsifier aqueous solution, and the feeding pump adds the emulsifier aqueous solution into the reactor at 5 ml / min. After the emulsifier aqueous solution is added, deionized water at 85-95° C. is added at 5 ml / min through a feed pump, and the stirring speed is increased to 300 rpm. When phase inversion occurs, the speed is reduced to 80 rpm, and deionized water is continued to be added to adjust the solid content to 50%. The temperature is lowered to below 40° C. and filtered through a 100-mesh stainless steel filter to obtain rosin ester emulsion ER8 with a solid content of about 50%, an average particle size of less than 0.6 μm, and a viscosity of less than 200 mPa.S. The storage period is greater than 180 days at 5-40° C.

[0058] Performance Testing

[0059] 1. At room temperature, the rosin ester emulsions ER3, ER4, ER5, ER6, ER7, and ER8 in the above examples were respectively added to the commercially available acrylic pressure-sensitive adhesive emulsion to complete compounding. The added amount was 5% of the mass of the acrylic pressure-sensitive adhesive emulsion. Stir for 30 minutes to obtain acrylic pressure-sensitive adhesive emulsions B / C / D / E / F / G, respectively. A was a pure acrylic pressure-sensitive adhesive emulsion.

[0060] Seven acrylic pressure-sensitive adhesive latexes, A, B, C, D, E, F, and G, were coated on 50 μm thick PET films using a four-sided applicator to prepare PET tapes with a film thickness of about 25 μm. After standing at room temperature for 24 hours, the 180° peel strength was tested using a LK-103B high and low temperature material tensile testing machine (Dongguan Likong Instrument Technology Co., Ltd.) at 25°C and -10°C in a box environment according to "GB / T 2792-2014 Test method for peel strength of adhesive tapes"; the initial adhesion was tested according to "GB / T 31125-2014 Test method for initial adhesion of adhesive tapes - ring method"; and the room temperature adhesion was tested using a LK-601B constant temperature tape adhesion tester (Dongguan Likong Instrument Technology Co., Ltd.) according to "GB / T 4851-2014 Test method for adhesion of adhesive tapes". The test results are shown in the table.

[0061] Table 2 Adhesive properties of rosin glycerol ester emulsion modified water-based acrylic ester pressure-sensitive adhesive emulsion

[0062]

[0063] From the above table, we can see that the rosin ester emulsion with vegetable oil added improves the bonding performance of the water-based pressure-sensitive adhesive under low temperature conditions without sacrificing the tackifying properties of the tackifying resin emulsion for the water-based pressure-sensitive adhesive at room temperature, and both the initial tack and peel strength of the adhesive are improved.

[0064] 2. The melt viscosity of the rosin ester emulsions of Examples 3 to 8 was measured. In the rosin ester emulsion products to which biomass oil was added, the melt viscosity decreased significantly. The results are shown in Table 3 below.

[0065] Table 3 Melt viscosity of rosin resin

[0066]

[0067]

[0068] From the above table, we can see that biomass oil, as a flux and bio-based plasticizer, effectively reduces the temperature required for resin melting and reduces the melt viscosity. The reduction in viscosity is conducive to improving the emulsification efficiency and thus improving the quality of the emulsion. On the other hand, the decrease in melt viscosity can also reduce production energy consumption and improve production efficiency.

[0069] 3. Bettersize 2600 laser particle size distribution analyzer (wet method) (Dandong Bettersize Instrument Co., Ltd.) measured the particle size distribution of the rosin ester emulsions of Examples 1 to 8. The results are shown in Table 4 and Figures 2 to 8 shown.

[0070] Table 4 Emulsion particle size distribution

[0071]

[0072] As can be seen from the above table, the addition of some biomass significantly reduces the average volume particle size of the rosin ester emulsion, especially the average volume particle sizes of rosin glycerol ester (+5% cottonseed oil) emulsion ER5 of Example 5, rosin glycerol ester (+10% cottonseed oil) emulsion ER6 of Example 6, and rosin glycerol ester (+20% cottonseed oil) emulsion ER7 of Example 7 are 0.309, 0.375 and 0.377, respectively, which are significantly lower than that of Example 3 without adding vegetable oil, and the D90 of rosin glycerol ester (+5% cottonseed oil) emulsion ER5 of Example 5 is less than 0.4μm, and the D90 of Examples 6 and 7 are 0.463μm and 0.473μm, respectively, which are significantly lower than Example 3.

[0073] Although the embodiments of the present invention have been disclosed above, they are not limited to the applications listed in the specification and the embodiments. They can be applied to various fields suitable for the present invention. For those familiar with the art, additional modifications can be easily realized.

Claims

1. A method for preparing an environmentally friendly rosin ester emulsion, characterized in that: include: Cardanol polyoxyethylene ether phosphate, alkyl glucoside APG1214, sodium lauroylbenzene sulfonate and deionized water are mixed uniformly at room temperature to prepare an emulsifier aqueous solution; rosin ester and a certain amount of biomass oil are mixed, heated and melted, and the emulsifier aqueous solution is added and mixed uniformly; deionized water is then added for emulsification, and after phase inversion occurs, deionized water is added to adjust the solid content, the temperature is lowered, and the rosin ester emulsion is obtained by filtering; In parts by weight, the rosin ester is 250 parts, the biomass oil is 5-50 parts, the cardanol polyoxyethylene ether phosphate is 10-30 parts, the alkyl glucoside APG1214 is 3-15 parts, the sodium lauroyl benzene sulfonate is 1-10 parts, and some deionized water; The rosin ester is rosin glycerol ester.

2. The method for preparing the environmentally friendly rosin ester emulsion according to claim 1, characterized in that: The weight parts of biomass oil are 12.5 parts, 25 parts or 50 parts.

3. The method for preparing the environmentally friendly rosin ester emulsion according to claim 1, characterized in that: The biomass oil is a biomass oil with a solidification point of ≤10°C and a decomposition temperature of ≥200°C.

4. The method for preparing the environmentally friendly rosin ester emulsion according to claim 1, characterized in that: The softening point of the rosin ester is 85°C to 95°C.

5. The method for preparing the environmentally friendly rosin ester emulsion according to claim 1, characterized in that: The temperature at which the rosin ester and the biomass oil are mixed and heated is 120°C to 180°C.

6. The method for preparing the environmentally friendly rosin ester emulsion according to claim 1, characterized in that: The molten rosin ester is stirred until transparent, and the emulsifier aqueous solution is heated to 60-90° C. and then added and mixed; the temperature of the deionized water is 85-95° C.

7. Use of the rosin ester emulsion prepared by the preparation method according to claim 1 in the preparation of pressure-sensitive adhesive emulsion.

8. Use of the rosin ester emulsion prepared by the preparation method according to claim 1 in the preparation of acrylic pressure-sensitive adhesive emulsion.

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