Novel wetting agent as well as preparation method and application thereof
The twin structural surfactant generated by the reaction of butyndiol tetraethoxy ether and linear siloxane solves the problem that existing wetting agents cannot take into account water solubility, surface tension and defoaming properties, and realizes a new wetting agent with multiple excellent properties, including good water solubility, low surface tension and unstable foam characteristics.
Patent Information
- Application Number
- CN202510140398.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-08
- Publication Date
- 2025-05-13
AI Technical Summary
Existing wetting agents cannot take into account water solubility, surface tension and defoaming properties, and usually require addition of other additives for supplementation or weakening.
A twin-structure bimini surfactant produced by the reaction of butyndeglycol tetraethoxy ether and linear siloxane was prepared by controlling the content proportion and reaction conditions of the raw materials, a new wetting agent with good water solubility, low static and dynamic surface tension, and unstable bubble and bursting ability were prepared.
The multiple excellent properties of the wetting agent are achieved, including good water solubility, low surface tension, rapid wetting of substrates, low foam generation and unstable foam characteristics, and there is no need to be combined with defoaming agents and has lower cost of use.
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Figure CN119978015A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of wetting agents, and in particular to a novel wetting agent and a preparation method and application thereof. Background Art
[0002] With the acceleration of urbanization and the rapid development of industry, the use of coatings is increasing. At the same time, as environmental protection requirements become more stringent, water-based additives, as a low-volatile organic compound, are widely used in paints, coatings, glues, printing, solar energy and other fields. From the perspective of environmental protection and health, water-based additives have gradually replaced traditional organic solvents and become the first choice for many industries, and all of this is inseparable from the contribution of additives. For example, as an indispensable component of coating production, coating additives can not only improve the production process and improve product quality in coating production, but also give coatings special functions, effectively improving coating construction conditions.
[0003] Common additives include wetting agents, which are chemical substances that can reduce the surface tension of liquids and promote the spreading and penetration of liquids on solid surfaces. Traditional wetting agents are mainly divided into surfactants, polymers and inorganic salts. Surfactants are the most widely used and have the best performance, but they often have a single function during application, or the surface tension is not enough, or the foam is too high, or the foam stability is strong, or the ability to reduce dynamic surface tension is poor, etc., and they cannot take into account multiple performances. Usually, other additives (such as defoamers) need to be added to supplement or weaken them.
[0004] In view of this, it is indeed necessary to provide a technical solution to the above problems. Summary of the invention
[0005] One of the purposes of the present invention is to provide a new wetting agent to solve the problem that the current wetting agent cannot take into account the water solubility, surface tension and defoaming performance.
[0006] In order to achieve the above object, the present invention adopts the following technical solutions:
[0007] A new wetting agent, calculated by mass percentage 100%, comprises the following raw materials:
[0008] Butynediol tetraethoxy ether 57%~60.9%,
[0009] Straight chain siloxane 39% to 42.9%,
[0010] Platinum-based catalyst 0.005% to 0.1%;
[0011] The number of silicon atoms in the linear siloxane is 3 to 7, and the structural formula of butynediol tetraethoxy ether is any of the following:
[0012] HO-CH2-CH2-O-CH2-C≡C-CH2-O-CH2-CH2-OH;
[0013] HO-(C2H4O)2-CH2-C≡C-CH2-(C2H4O)2-OH;
[0014] HO-(C2H4O)3-CH2-C≡C-CH2-(C2H4O)3-OH;
[0015] HO-(C2H4O)2-CH2-C≡C-CH2-O-CH2-CH2-OH.
[0016] Preferably, the structural formula of butynediol tetraethoxy ether is: HO-(C2H4O)2-CH2-C≡C-CH2-(C2H4O)2-OH.
[0017] Preferably, the linear siloxane is any one of heptamethyltrisiloxane, nonamethyltetrasiloxane, undecamethylpentasiloxane, tridecamethylhexasiloxane and pentadecylheptasiloxane; and the platinum-based catalyst is chloroplatinic acid.
[0018] Preferably, the raw materials included are 100% by mass:
[0019] Butynediol tetraethoxy ether 58% to 59.95%;
[0020] Straight chain siloxane 40% to 41.95%;
[0021] Platinum-based catalyst 0.005% to 0.05%.
[0022] The second object of the present invention is to provide a method for preparing the novel wetting agent described above, comprising the following steps:
[0023] S1, mixing and stirring a linear siloxane and a portion of butynediol tetraethoxy ether, and heating to 140° C. to 149° C., and then adding a platinum-based catalyst;
[0024] S2. After the temperature reaches 150°C to 160°C, add the remaining butynediol tetraethoxy ether and control the reaction temperature to 145°C to 165°C;
[0025] S3. After the reaction, ripen for 1 to 3 hours, cool down, and complete the preparation of the new wetting agent.
[0026] Preferably, butynediol tetraethoxy ether is obtained by addition reaction of butynediol and ethylene oxide at 100°C to 125°C in the presence of a base catalyst KOH; the raw material mass ratio of butynediol to ethylene oxide is (32.6 to 33.0):(67 to 67.4).
[0027] Preferably, in step S1, the amount of butynediol tetraethoxy ether added is 5% to 25% of the total amount added; and the stirring speed is 60 to 80 r / min.
[0028] Preferably, in step S2, the remaining butynediol tetraethoxy ether is added dropwise.
[0029] Preferably, the dripping flow rate is 28-32 kg / min.
[0030] The third object of the present invention is to provide an application of the novel wetting agent described above or the novel wetting agent prepared by the preparation method of the novel wetting agent described above in any of coatings, paints, glues, printing and solar energy.
[0031] The beneficial effects of the present invention are as follows: the wetting agent provided by the present invention is a twin-type surfactant having a twin structure generated by the reaction of butynediol tetraethoxy ether and linear siloxane. Compared with the traditional allyl monomer wetting agent, the wetting agent of the present invention combines the hydrophilic properties of butynediol tetraethoxy ether on the one hand, showing good water solubility, and on the other hand combines the wettability and low surface tension advantages of linear siloxane, can reduce static surface tension, and obtain the performance of reducing dynamic surface tension that pure linear siloxane does not have. The wetting agent can quickly complete the migration from the bulk phase to the interface in the aqueous system, achieve the purpose of quickly reducing the dynamic surface tension, and can wet the substrate more efficiently and quickly. In addition, compared with the shortcomings of traditional allyl monomer wetting agents that are easy to foam, have strong foam stability, and often need to be used in combination with defoamers, the new wetting agent of the present invention has a unique twin structure, which greatly reduces the generation of foam, and at the same time presents the characteristics of unstable foam, has a certain ability to break and defoam, and can show multiple excellent performances without being used in combination with defoamers. BRIEF DESCRIPTION OF THE DRAWINGS
[0032] Figure 1 This is a surface tension trend diagram of the wetting agent in Example 1 of the present invention.
[0033] Figure 2 This is a surface tension trend diagram of the wetting agent in Comparative Example 1 of the present invention. DETAILED DESCRIPTION
[0034] In order to make the technical solutions and advantages of the present invention more clear, the present invention and its beneficial effects are described in further detail below, but the embodiments of the present invention are not limited thereto.
[0035] The wetting agent of the present invention can be used as an auxiliary agent in any of coatings, paints, glues, printing and solar energy. Of course, it can also be used in other fields that require a wetting agent, which is not limited here.
[0036] The novel wetting agent comprises the following raw materials, calculated by mass percentage of 100%, including 57% to 60.9% of butynediol tetraethoxy ether, 39% to 42.9% of linear siloxane, and 0.005% to 0.1% of a platinum-based catalyst; wherein the number of silicon atoms in the linear siloxane is 3 to 7, and the structural formula of butynediol tetraethoxy ether is HO-(C2H4O)2-CH2-C≡C-CH2-(C2H4O)2-OH.
[0037] The wetting agent of the present invention is obtained by reacting butynediol tetraethoxy ether and straight-chain siloxane. The carbon bond in the alkynyl group is broken and the siloxane is grafted, rather than grafting the siloxane to the end of butynediol tetraethoxy ether. The unique twin structure formed by the wetting agent not only retains the excellent properties of the two reaction raw materials, but also has good compatibility in both aqueous systems and oily systems, and has a wider range of application fields; and also obtains a superior foam breaking ability. In practical applications, the use of a defoaming agent can be omitted, and the use cost is lower.
[0038] Specifically, the number of silicon atoms in the linear siloxane may be 3, 4, 5, 6 or 7.
[0039] More specifically, the straight-chain siloxane may be any one of heptamethyltrisiloxane, nonamethyltetrasiloxane, undecamethylpentasiloxane, tridecamethylhexasiloxane and pentadecylheptasiloxane; preferably, the straight-chain siloxane may be heptamethyltrisiloxane, which is prepared from high-quality hydrogenated silicone oil and has the advantages of super wettability and low surface tension. It is a lipophilic substance and although it is insoluble in water, after combining with tetraethoxy butynediol, the wetting agent can exhibit both hydrophilic and lipophilic properties.
[0040] Using butynediol tetraethoxy ether as the raw material for the reaction, the inventors found that adding four ethylene oxides to butynediol can obtain a molecular structure with better performance. Compared with the grafted long-chain siloxane, the twin structure of the present invention not only has better stability, but also has better performance in water solubility, surface tension, and defoaming ability. In particular, the grafting reaction with heptamethyltrisiloxane can obtain a wetting agent with better performance in water solubility, surface tension, and defoaming performance, taking into account the multiple properties required by the wetting agent without adding other additives for supplementation or weakening.
[0041] In order to obtain a wetting agent with a unique twin structure, the content ratio of the raw materials used must also be controlled. Specifically, the mass ratio of butynediol tetraethoxy ether can be 57% to 58%, 58% to 59%, 59% to 59.9% or 59.9% to 60.9%; the mass ratio of linear siloxane is 39% to 40.9%, 40.9% to 41.9% or 41.9% to 42.9%; the mass ratio of platinum-based catalyst is 0.005% to 0.009%, 0.009% to 0.015%, 0.015% to 0.05% or 0.05% to 0.1%.
[0042] Preferably, the mass proportion of butynediol tetraethoxy ether is 58% to 59.95%, the mass proportion of linear siloxane is 40% to 41.95%, and the mass proportion of platinum-based catalyst is 0.005% to 0.05%. More preferably, the mass proportion of butynediol tetraethoxy ether is 58.4% to 59%, the mass proportion of linear siloxane is 41% to 41.8%, and the mass proportion of platinum-based catalyst is 0.009% to 0.015%.
[0043] By controlling the proportion of each raw material content within the above range, any performance of the wetting agent will not be affected by excessive or insufficient content of a certain substance. This ensures the balance of multiple properties of the wetting agent while giving it more unique properties, such as reducing dynamic surface tension and bubble breaking properties.
[0044] One of the raw materials of the present invention is butynediol tetraethoxy ether, which belongs to acetylenic alcohol ethers, and the acetylenic bond is larger than the traditional double-bond olefin bond energy, and the required reaction temperature is high, and the boiling point of linear siloxane is relatively low, and the problem of bumping is prone to occur, resulting in butynediol tetraethoxy ether and linear siloxane synthesis difficulty being greater, and strict temperature control is required in the synthetic process. It should be noted that the reactor as the reaction should clean the bottom of the kettle before the reaction to prevent the occurrence of other chemical reactions, and in addition to avoid moisture affecting the reaction, the bottom of the kettle needs to be heated and dried. Before the production preparation at the same time, it is also necessary to detect other performances of the reactor, such as the pipeline blocking problem, to ensure production safety.
[0045] Based on this, the present invention provides a method for preparing the novel wetting agent, comprising the following steps:
[0046] S1, mixing and stirring a linear siloxane and a portion of butynediol tetraethoxy ether, and heating to 140° C. to 149° C., and then adding a platinum-based catalyst;
[0047] S2. After the temperature reaches 150°C to 160°C, add the remaining butynediol tetraethoxy ether and control the reaction temperature to 145°C to 165°C;
[0048] S3. After the reaction, ripen for 1 to 3 hours, cool down, and complete the preparation of the new wetting agent.
[0049] The inventors have concluded through multiple experimental studies that butynediol tetraethoxy ether adopts a distributed addition method, and after the temperature rises to 140°C to 149°C, a platinum-based catalyst is added to carry out the first reaction. The reaction is an exothermic reaction, but because the boiling point of linear siloxane is lower than 145°C, after the system temperature rises to the boiling point of linear siloxane during the reaction, the linear siloxane begins to boil and generate gas pressure, forming a reflux. During the reflux process, the linear siloxane will take away part of the heat of the system, causing the temperature to drop, which is exactly the opposite of the exothermic reaction. However, in general, the system temperature during the first reaction is on an upward trend. After the temperature reaches 150°C to 160°C, the remaining butynediol tetraethoxy ether is added to increase the concentration of the reactants to increase the reaction rate. However, in order to control the reaction temperature to be continuously maintained between 145°C and 165°C, the remaining butynediol tetraethoxy ether is added gradually so that the reaction temperature can be adjusted at any time. This can more accurately and safely control the reaction process and ensure the performance of the generated wetting agent.
[0050] The wetting agent prepared by the method of the present invention has a higher synthesis reaction temperature and is more stable. It can stably exist at high temperatures of 200°C and below -30°C. However, traditional allyl monomer wetting agents are often easily decomposed at 140°C and have relatively poor storage stability.
[0051] The preparation process of the present invention does not contain VOC, is very environmentally friendly, and is more green, safe and environmentally friendly.
[0052] Preferably, in step S1, when the system is heated to 140°C to 142°C, the feed port of the reactor can be opened to add the platinum-based catalyst, and then after the temperature reaches 150°C to 155°C, the remaining butynediol tetraethoxy ether can be added.
[0053] In some embodiments, butynediol tetraethoxy ether is obtained by addition reaction of butynediol and ethylene oxide at 100°C to 125°C under the action of a base catalyst; the base catalyst may be KOH. The hydrophilicity of the generated butynediol tetraethoxy ether may be improved by modifying butynediol with ethylene oxide; the raw material mass ratio of butynediol and ethylene oxide is (32.6 to 33.0): (67 to 67.4). Specifically, the raw material mass ratio of butynediol and ethylene oxide includes but is not limited to: 32.6:67.4, 32.7:67.3, 32.8:67.2%, 32.9%:67.1 or 33:67. The butynediol tetraethoxy ether selected by the present invention is preferably butynediol with 4 ethylene oxides added thereto, and the synthesized butynediol tetraethoxy ether has a better molecular structure, and the structural formula is HO-(C2H4O)2-CH2-C≡C-CH2-(C2H4O)2-OH.
[0054] In some embodiments, in step S1, the amount of butynediol tetraethoxy ether added is 5% to 25% of the total amount added; in the first reaction, the amount of butynediol tetraethoxy ether added is controlled to be less, on the one hand, the system reaction will not be too violent, affecting the production of the wetting agent; on the other hand, due to the influence of the boiling point of the reaction raw materials and the reaction temperature on each other, a small amount of butynediol tetraethoxy ether is pre-reacted, and the subsequent gradual addition of the remaining acetylene glycol ether compounds is equivalent to supplementing a part of the raw materials, promoting the forward reaction and improving production efficiency. Preferably, the amount of butynediol tetraethoxy ether added is 5% to 15% of the total amount added. Further preferably, the amount of butynediol tetraethoxy ether added is 8% to 12% of the total amount added.
[0055] In addition, the stirring speed is controlled to 60-80 r / min to better promote the uniformity of the system reaction.
[0056] In some embodiments, in step S2, the remaining butynediol tetraethoxy ether is added dropwise. Compared with directly adding all the remaining butynediol tetraethoxy ether or gradually flowing in, the dropwise addition can more strictly control the reaction temperature. Once the reaction temperature of the system is detected to be lower than 145°C, the addition of butynediol tetraethoxy ether can be suspended, and the temperature can be raised to the reaction temperature before adding, thereby avoiding the problem of insufficient reaction and ensuring the product quality of the generated wetting agent.
[0057] After many explorations, the addition flow rate of the remaining butynediol tetraethoxy ether was controlled between 28 and 32 kg / min. The reaction temperature could be strictly controlled while ensuring production efficiency.
[0058] The present invention and its beneficial effects will be described in further detail below in conjunction with specific embodiments and the accompanying drawings, but the embodiments of the present invention are not limited thereto.
[0059] Example 1
[0060] A new type of wetting agent, calculated by mass percentage of 100%, comprises the following raw materials: 58.5% of butynediol tetraethoxy ether, 41.49% of linear siloxane, and 0.01% of platinum-based catalyst;
[0061] Among them, the structural formula of butynediol tetraethoxy ether is HO-(C2H4O)2-CH2-C≡C-CH2-(C2H4O)2-OH, hereinafter referred to as A1; the straight-chain siloxane is heptamethyltrisiloxane, produced by Zhejiang Runhe Silicone New Materials Co., Ltd., hereinafter referred to as B1; the platinum-based catalyst is chloroplatinic acid.
[0062] The preparation method of butynediol tetraethoxy ether is as follows: 32.8 kg of butynediol and 67.2 kg of ethylene oxide are subjected to addition reaction at 110° C. under the action of KOH catalyst to obtain butynediol tetraethoxy ether.
[0063] The preparation method of the novel wetting agent is:
[0064] According to the above-mentioned feed ratio, 414.9 kg of straight-chain siloxane and 58.5 kg (10%) of butynediol tetraethoxy ether were added into the reactor, stirred and mixed at a speed of 70 r / min. After the temperature in the reactor rose to 140°C, the feed port was opened and 0.1 kg of platinum-based catalyst was added; then when the temperature reached 150°C, the flow rate was controlled at 30 kg / min to dropwise add the remaining butynediol tetraethoxy ether, and the reaction temperature was controlled to be 145°C-165°C. The dropwise addition could be paused appropriately according to the temperature in the reactor. If the temperature dropped, the dropwise addition must be stopped to heat up before adding dropwise again; after the reaction was completed, it was aged for 2 hours, then cooled to 70°C, filtered and packaged to complete the preparation of the new wetting agent.
[0065] Example 2
[0066] The difference from Example 1 is that the raw material composition used in this example is different, that is, based on 100% by mass, 58% of tetraethoxy butynediol, 41.99% of linear siloxane, and 0.01% of platinum-based catalyst; the rest can be found in Example 1 and will not be repeated here.
[0067] Example 3
[0068] Different from Example 1, the raw material composition and preparation method used in this example are different, based on 100% by mass, 57% of butynediol tetraethoxy ether, 42.9% of linear siloxane, and 0.1% of platinum-based catalyst;
[0069] The preparation method of butynediol tetraethoxy ether is as follows: 32.6 kg of butynediol and 67.4 kg of ethylene oxide are subjected to an addition reaction at 100° C. in the presence of an alkali catalyst to obtain butynediol tetraethoxy ether.
[0070] The preparation method of this embodiment is:
[0071] According to the above-mentioned feed ratio, 429 kg of straight-chain siloxane and 57 kg (10%) of butynediol tetraethoxy ether were added into the reactor, stirred and mixed at a speed of 60 r / min. After the temperature in the reactor rose to 145°C, 1 kg of platinum-based catalyst was added by opening the feed port; then when the temperature reached 155°C, the flow rate was controlled at 28 kg / min to dropwise add the remaining butynediol tetraethoxy ether, and the reaction temperature was controlled at 145°C to 165°C. The dropwise addition could be paused appropriately according to the temperature in the reactor. If the temperature dropped, the dropwise addition must be stopped to heat up before adding dropwise; after the reaction was completed, it was aged for 1 hour, then cooled to 70°C, filtered and packaged to complete the preparation of the new wetting agent.
[0072] For the rest, please refer to Example 1 and will not be described again here.
[0073] Example 4
[0074] The difference from Example 1 is that the raw material composition used in this example is different, that is, based on 100% by mass, 59.95% of tetraethoxy butynediol, 40.04% of linear siloxane, and 0.01% of platinum-based catalyst; the rest can be found in Example 1 and will not be repeated here.
[0075] Example 5
[0076] Different from Example 1, the raw material composition used in this example is different, based on 100% by mass, 60.9% of butynediol tetraethoxy ether, 39% of linear siloxane, and 0.1% of platinum-based catalyst;
[0077] The preparation method of butynediol tetraethoxy ether is as follows: 33 kg of butynediol and 67 kg of ethylene oxide are subjected to an addition reaction at 125° C. in the presence of an alkali catalyst to obtain butynediol tetraethoxy ether.
[0078] The preparation method of this embodiment is:
[0079] According to the above-mentioned feed ratio, 390 kg of straight-chain siloxane and 60.9 kg (10%) of butynediol tetraethoxy ether were added into the reactor, stirred and mixed at a speed of 80 r / min. After the temperature in the reactor rose to 149°C, the feed port was opened and 1 kg of platinum-based catalyst was added; then when the temperature reached 160°C, the flow rate was controlled at 32 kg / min to dropwise add the remaining butynediol tetraethoxy ether, and the reaction temperature was controlled to be 145°C-165°C. The dropwise addition could be paused appropriately according to the temperature in the reactor. If the temperature dropped, the dropwise addition must be stopped to heat up before adding dropwise again; after the reaction was completed, it was aged for 3 hours, then cooled to 70°C, filtered and packaged to complete the preparation of the new wetting agent.
[0080] For the rest, please refer to Example 1 and will not be described again here.
[0081] Example 6
[0082] The difference from Example 1 is that the linear siloxane used in this example is undecamethylpentasiloxane, hereinafter referred to as B2. The rest is as in Example 1 and will not be described again.
[0083] Example 7
[0084] The difference from Example 1 is that the linear siloxane used in this example is pentadecylheptasiloxane, hereinafter referred to as B3. The rest is as in Example 1 and will not be described again.
[0085] Example 8
[0086] The difference from Example 1 is that in the preparation method of the novel wetting agent, the first feeding amount of butynediol tetraethoxy ether is 25% of the total amount, and the rest can be found in Example 1 and will not be described again.
[0087] Example 9
[0088] The difference from Example 1 is that in the preparation method of the novel wetting agent, the first feeding amount of butynediol tetraethoxy ether is 50% of the total amount, and the rest can be referred to Example 1 and will not be described again.
[0089] Example 10
[0090] The difference from Example 1 is that in the preparation method of the novel wetting agent, the flow rate of the second feeding of butynediol tetraethoxy ether is 60 kg / min. The rest can be found in Example 1 and will not be described again.
[0091] Comparative Example 1
[0092] Traditional allyl alcohol polyether modified 245 (TEGO-245 produced by Evonik of Germany) is selected, hereinafter referred to as D1.
[0093] Comparative Example 2
[0094] The difference from Example 1 is that the linear siloxane used in this comparative example is tritrismethylhexasiloxane, hereinafter referred to as B4. The rest is as in Example 1 and will not be described again.
[0095] Comparative Example 3
[0096] The difference from Example 6 is that the linear siloxane used in this comparative example is tritrismethylhexasiloxane, hereinafter referred to as B4. The rest is referred to Example 6 and will not be described again.
[0097] Comparative Example 4
[0098] Different from Example 1, in the preparation method of the new wetting agent, the linear siloxane, butynediol tetraethoxy ether and platinum-based catalyst are directly added into the reaction kettle at one time, and the reaction is carried out at 145° C. to 165° C. The rest can be referred to Example 1 and will not be repeated here.
[0099] Comparative Example 5
[0100] The difference from Example 1 is that when the temperature reaches 150°C, the remaining butynediol tetraethoxy ether is added dropwise at a flow rate of 30 kg / min; after the reaction is completed, the mixture is aged for 2 hours, then cooled to 70°C, filtered and packaged, and the preparation of the new wetting agent is completed. The rest can be referred to Example 1, which will not be repeated here.
[0101] The wetting agents obtained in the above Examples 1 to 10 and Comparative Examples 1 to 5 were dissolved in an aqueous solution at a concentration of 0.1%, and tested using a liquid tension analyzer SITApro line t15, wherein the rate of decrease of the surface tension value = (surface tension initial value - surface tension value corresponding to the bubble life time) / surface tension initial value.
[0102] The test results are shown in Table 1 and Figures 1-2 .
[0103] Table 1 Surface tension data table
[0104]
[0105] From the above Table 1 and Figures 1-2 It can be seen from the comparison that compared with the traditional allyl alcohol polyether modified 245, the new wetting agent provided by the present invention not only has a lower surface tension value, but also can quickly reduce the dynamic surface tension. In particular, when the appropriate reaction conditions are controlled, the prepared wetting agent has high purity, not only the static surface tension can reach 20 dynes, but also can effectively reduce the dynamic surface tension, so as to achieve the purpose of quickly wetting the substrate, which is very suitable for some productions with wetting time requirements, such as the ink printing industry.
[0106] In addition, it can be seen from the comparison of Examples 1 to 5 that different raw material ratios will affect the surface tension properties of the generated wetting agent. Preferably, the mass proportion of butynediol tetraethoxy ether is controlled to be 58% to 59.95%, and the mass proportion of linear siloxane is 40% to 41.95% to obtain a relatively purer and more stable twin structure wetting agent. The selected raw materials are different, and the structure of the generated wetting agent is different. As can be seen from the comparison of Examples 1, 6, 7 and Comparative Example 2, adding four ethylene oxides to butynediol can obtain butynediol tetraethoxy ether with a better molecular structure, and then the wetting agent generated by combining with heptamethyl trisiloxane not only has a low initial surface tension value, but also the surface tension value can be reduced to 49% at 0.08s.
[0107] It should also be noted that, because the reaction between tetraethoxy butynediol and linear siloxane is very violent, and there is a correlation between the boiling point of the reaction raw materials and the reaction temperature, it is necessary to strictly control the production steps and the reaction temperature so that the structure and performance of the wetting agent obtained are more stable and excellent, as shown in the comparison of the test results of Examples 1, 8 to 10 and Comparative Examples 4 to 5.
[0108] In addition, to further prove that the wetting agent of the present invention has the advantage of low and unstable foam, the foam height of Example 1, Comparative Example 1 and Comparative Example 2 was tested. The test results are shown in Table 2 below.
[0109] Table 2 Foam height and time relationship
[0110]
[0111] It can be seen from the above test results that the wetting agent provided by the present invention generates low foam and is unstable. In practical applications, it can be used without the assistance of a defoaming agent. Not only is the production cost low, but the wetting agent of the present invention is also more suitable for some special low-foam use requirements.
[0112] According to the disclosure and teaching of the above description, those skilled in the art to which the present invention belongs can also change and modify the above embodiment. Therefore, the present invention is not limited to the above specific embodiment, and any obvious improvement, replacement or modification made by those skilled in the art on the basis of the present invention belongs to the protection scope of the present invention. In addition, although some specific terms are used in this specification, these terms are only for the convenience of description and do not constitute any limitation to the present invention.
Claims
1. A novel wetting agent, characterized in that: Calculated by mass percentage 100%, including the following raw materials: Butynediol tetraethoxy ether 57%~60.9%, Straight chain siloxane 39% to 42.9%, Platinum-based catalyst 0.005% to 0.1%; Among them, the number of silicon atoms in the straight-chain siloxane is 3 to 7, and the structural formula of butynediol tetraethoxy ether is HO-(C2H4O)2-CH2-C≡C-CH2-(C2H4O)2-OH.
2. The novel wetting agent according to claim 1, characterized in that The linear siloxane is any one of heptamethyltrisiloxane, nonamethyltetrasiloxane, undecamethylpentasiloxane, tridecamethylhexasiloxane and pentamethylheptasiloxane; and the platinum-based catalyst is chloroplatinic acid.
3. The novel wetting agent according to claim 1 or 2, characterized in that: Calculated by mass percentage 100%, the raw materials included are: Butynediol tetraethoxy ether 58% to 59.95%; Straight chain siloxane 40% to 41.95%; Platinum-based catalyst 0.005% to 0.05%.
4. A method for preparing the novel wetting agent according to any one of claims 1 to 3, characterized in that: The following steps are involved: S1, mixing and stirring a linear siloxane and a portion of butynediol tetraethoxy ether, and heating to 140° C. to 149° C., and then adding a platinum-based catalyst; S2. After the temperature reaches 150°C to 160°C, add the remaining butynediol tetraethoxy ether and control the reaction temperature to 145°C to 165°C; S3. After the reaction, mature for 1 to 3 hours and cool down to complete the preparation of the new wetting agent.
5. The method for preparing the novel wetting agent according to claim 4, characterized in that: Butynediol tetraethoxy ether is obtained by addition reaction of butynediol and ethylene oxide at 100-125°C in the presence of an alkali catalyst; the raw material mass ratio of butynediol to ethylene oxide is (32.6-33.0):(67-67.4).
6. The method for preparing the novel wetting agent according to claim 4, characterized in that: In step S1, the amount of butynediol tetraethoxy ether added is 5% to 25% of the total amount added; and the stirring speed is 60 to 80 r / min.
7. The method for preparing the novel wetting agent according to claim 4, characterized in that: In step S2, the remaining butynediol tetraethoxy ether is added dropwise.
8. The method for preparing the novel wetting agent according to claim 7, characterized in that: The flow rate of the dropwise addition is 28-32 kg / min.
9. Use of the novel wetting agent according to any one of claims 1 to 3 or the novel wetting agent prepared by the preparation method of the novel wetting agent according to any one of claims 4 to 8 in coatings, paints, glues, printing and solar energy.