TW201710481A - Fireproof material having woody material combined with aerogel and manufacturing method thereof having excellent fire resistance and capable of passing the lowest oxygen content test in burning - Google Patents
Fireproof material having woody material combined with aerogel and manufacturing method thereof having excellent fire resistance and capable of passing the lowest oxygen content test in burning Download PDFInfo
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本發明係有關於一種具有極佳耐熱、防火功能之防火材結構及其製造方法。The invention relates to a fireproof material structure with excellent heat resistance and fireproof function and a manufacturing method thereof.
按，氣凝膠擁有許多的特殊性質，如低密度、高孔隙率、高比表面積以及低熱傳導係數。目前針對氣凝膠的製造方法係以溶膠凝膠合成法，由烷氧化矽類(Alkoxysilane)或正矽酸甲酯等前驅物與含水有機溶劑進行混合後，添加酸觸媒，進行水解反應(Hydrolysis)。水解一定時間後，再添加鹼觸媒，進行縮合反應(Condensation)，在縮合反應期間稱為溶膠溶液。在溶膠溶液中的二氧化矽分子繼續進行縮合聚集，逐漸形成二氧化矽凝膠。According to the aerogel, there are many special properties such as low density, high porosity, high specific surface area and low heat transfer coefficient. At present, a method for producing an aerogel is a sol-gel synthesis method in which a precursor such as Alkoxysilane or methyl ortho-nonanoate is mixed with an aqueous organic solvent, and then an acid catalyst is added to carry out a hydrolysis reaction ( Hydrolysis). After hydrolysis for a certain period of time, a base catalyst is added to carry out a condensation reaction (Condensation), which is referred to as a sol solution during the condensation reaction. The cerium oxide molecules in the sol solution continue to undergo condensation condensation and gradually form a cerium oxide gel.
傳統氣凝膠溶液中，因含有大量的乙醇(酒精)分子，故其在乾燥製程期間會形成乙醇蒸氣，當乾燥環境中乙醇蒸氣達氣爆臨界值以上，對於結合以氣凝膠為主之各種製程，於工安上有極大的影響。In the traditional aerogel solution, because it contains a large amount of ethanol (alcohol) molecules, it will form ethanol vapor during the drying process. When the ethanol vapor reaches a critical value above the gas explosion in the dry environment, it is mainly combined with aerogel. Various processes have a great impact on the work safety.
傳統氣凝膠材料，因含有大量的水分子，故其乾燥製程需利用二氧化碳超臨界乾燥機進行乾燥，而製程條件係在溫度攝氏34度下以高壓，將液態二氧化碳轉變成超臨界條件，並利用超臨界二氧化碳將氣凝膠中水分子溶出乾燥。惟，此製程並無法轉換成為工業化之製程。Conventional aerogel materials contain a large amount of water molecules, so the drying process needs to be dried by a carbon dioxide supercritical dryer, and the process conditions are at a high pressure of 34 degrees Celsius to convert liquid carbon dioxide into supercritical conditions, and The water molecules in the aerogel are dissolved and dried using supercritical carbon dioxide. However, this process cannot be converted into an industrial process.
目前國內外一些有關氣凝膠材料專利的先前技術資料，略舉如下：Some prior art materials on aerogel material patents at home and abroad are as follows:
1.西元2011年10月4日所公告之美國第8029871號「生產二氧化矽氣凝膠塗層的方法」專利案，揭示二氧化矽氣凝膠塗料係由烷氧基矽烷和有機改性劑進行水解以及聚合所獲得濕的有機改性二氧化矽凝膠，利用超聲波處理所製備的形成有機改性二氧化矽凝膠形成有機改性的二氧化矽分散物，添加紫外線固化型樹脂和光聚合引發劑於此有機改性的二氧化矽分散物形成二氧化矽氣凝膠塗料液體，應用此塗料液體於基材上，然後照射紫外線於此塗層。1. Patent No. 8028871, "Method for Producing Cerium Oxide Aerogel Coating", published on October 4, 2011, reveals that cerium oxide aerogel coating is modified by alkoxy decane and organic The agent is subjected to hydrolysis and polymerization to obtain a wet organically modified cerium oxide gel, and an organically modified cerium oxide gel prepared by ultrasonic treatment is formed to form an organically modified cerium oxide dispersion, and an ultraviolet curing resin and light are added. Polymerization Initiator The organically modified ceria dispersion forms a ceria aerogel coating liquid, which is applied to a substrate and then irradiated with ultraviolet light to the coating.
2.中華民國97年9月1日所公開之發明第200835648號「多孔材料及其製備方法」專利案，係揭露：由烷氧化矽類或矽酸鹽類化合物與有機溶劑以溶膠凝膠法合成，並經改質劑改質而製得。亦提供一製作多孔結構材料的方法，包含：(a)混合烷氧化矽類或矽酸鹽類化合物與有機溶劑以溶膠凝膠法合成，並經改質劑改質而製得。係利用改質劑將多孔結構材料表面之親水官能基置換為疏水官能基，可降低其表面張力，以維持多孔結構。所製得之多孔結構材料，具低熱傳導係數、高孔隙率及高疏水性與自潔能力等特性。2. Patent No. 200835648, "Polyporous Materials and Preparation Methods" disclosed in the Republic of China on September 1, 1997, discloses a sol-gel method from an alkoxylated oxime or a phthalate compound and an organic solvent. Synthetic and prepared by upgrading the modifier. A method for producing a porous structural material is also provided, which comprises: (a) mixing an alkoxylated hydrazine or a phthalate compound with an organic solvent by a sol-gel method and modifying it by a modifier. The hydrophilic functional group on the surface of the porous structural material is replaced with a hydrophobic functional group by a modifier, and the surface tension thereof is lowered to maintain the porous structure. The porous structural material has the characteristics of low thermal conductivity, high porosity, high hydrophobicity and self-cleaning ability.
3.中華民國101年4月11日所公告之新型第M426798號「用於電子產品的阻熱裝置」專利案，係揭露：包含有一容置元件及至少一氣凝膠層。藉由使容置元件包覆氣凝膠層，並且搭配組合成各式阻熱裝置，以可有效發揮氣凝膠的眾多優點，如下：其一，熱傳導係數低，阻熱效果佳；其二，耐高溫的效果佳於現有之泡棉及橡膠等材料；其三，完全防水及防水氣，不會有受潮等問題；其四，薄型化後不會影響其阻熱能力。此外尚有重量輕、防火、防鹽害、防腐蝕、抗壓耐衝擊等優點，並可持續使用超過20年及重複使用，進而減少汰換成本。藉此解決現有阻熱裝置其阻熱效果不佳、不耐高溫及潮溼，並且無法薄型化的缺點。3. The new patent No. M426798, "Heat Resistant Device for Electronic Products", published on April 11, 101, discloses a package element and at least one aerogel layer. By covering the aerogel layer with the accommodating element and combining them into various heat-blocking devices, the advantages of the aerogel can be effectively utilized as follows: First, the heat transfer coefficient is low, and the heat-resisting effect is good; The effect of high temperature resistance is better than that of existing foam and rubber materials; thirdly, it is completely waterproof and waterproof, and there is no problem such as moisture; fourthly, it does not affect its heat resistance after thinning. In addition, it has the advantages of light weight, fireproof, salt-proof, anti-corrosion, anti-pressure and impact resistance, and can be used for more than 20 years and reused, thus reducing the cost of replacement. Therefore, the existing heat-resisting device has the disadvantages of poor heat-resistance, high temperature and humidity resistance, and inability to be thinned.
惟，上述該等專利前案並未有針對回收的木質材料結合氣凝膠製成防火材，以及所需的製造步驟及條件進行改良，也非減少製程中的工安問題，因此均未揭示出與本發明相同之技術特徵及功效。However, the above-mentioned patents do not disclose the fire-retardant materials for the recycled wood materials combined with aerogels, as well as the required manufacturing steps and conditions, and do not reduce the safety problems in the process. The same technical features and effects as the present invention are obtained.
爰此，有鑑於氣凝膠應用於隔熱或多孔吸附應用專利眾多，但尚無揭示有含浸於回收木屑中，用以結合製成一防火材的專利技術，因此本發明提出一種回收木屑結合氣凝膠製成之防火材及其製造方法，藉由結合多孔性矽酸鹽氣凝膠材料的高隔熱特性，以及回收木屑的低成本、高減碳、優異力學性質等特性，以達到利用回收木屑結合氣凝膠以製造防火材之目的。Therefore, in view of the numerous patents applied to the application of aerogels for thermal insulation or porous adsorption, there is no disclosure of a patented technique for impregnating recycled wood chips for combining a fireproof material. Therefore, the present invention proposes a combination of recycled wood chips. The fireproof material made of aerogel and the manufacturing method thereof are achieved by combining the high heat insulating property of the porous tantalum aerogel material, and the low cost, high carbon reduction, excellent mechanical properties and the like for recovering wood chips. The purpose of manufacturing fireproof materials is to use recycled wood chips in combination with aerogels.
故本發明提供一種木質材料結合氣凝膠之防火材製造方法，包括有：A.於一前驅物與一有機溶劑之混合溶液中加入一酸觸媒，使其產生水解反應而成為一氣凝膠溶液，該前驅物係為一烷氧化矽類或一正矽酸甲酯，該有機溶劑係以一水及一乙醇進行混合而成，該水及該乙醇的莫耳比含量範圍係為10比1至120比8，該前驅物的莫耳比含量占該混合溶液中的9%至16%，該有機溶劑的莫耳比含量占該混合溶液中的84%至91%，又該前驅物與該酸觸媒的莫耳比含量範圍係由1比0.001至1比0.1，使得該前驅物的莫耳比含量占該氣凝膠溶液中的9.1%至16.66%，該有機溶劑的莫耳比含量占該氣凝膠溶液中的83.33%至90.60%，該酸觸媒的莫耳比含量占該氣凝膠溶液中的0.003%至0.3%；B.於該氣凝膠溶液中加入一鹼觸媒水溶液，使其產生縮合反應而形成一氣凝膠水溶液，該鹼觸媒水溶液係由一鹼觸媒與一水溶液配置而成，該鹼觸媒與該水溶液的莫耳比含量範圍係為0.003比16至0.2比180，經縮合反應後之該氣凝膠水溶液中，該前驅物的莫耳比含量占該氣凝膠水溶液的0.32%至7.07%，該乙醇的莫耳比含量占該氣凝膠水溶液的1.61%至21.20%，而所含水溶液的莫耳比含量占該氣凝膠水溶液的70.67%至98.02%，該鹼觸媒的莫耳比含量係占該氣凝膠水溶液中的0.05%至1.06%；C.將一木質材料含浸於該氣凝膠水溶液，經凝膠化而產生一氣凝膠包覆該木質材料； D.使該木質材料乾燥後成型為一防火材。Therefore, the present invention provides a method for manufacturing a fireproof material of a wood material combined with an aerogel, comprising: A. adding an acid catalyst to a mixed solution of a precursor and an organic solvent to cause a hydrolysis reaction to become an aerogel a solution, the precursor is a lanthanum alkoxide or a methyl decanoate, the organic solvent is a mixture of monohydrate and ethanol, and the molar ratio of the water and the ethanol is 10 ratio. 1 to 120 to 8, the precursor has a molar ratio of 9% to 16% of the mixed solution, and the organic solvent has a molar ratio of 84% to 91% of the mixed solution, and the precursor The molar ratio of the acid catalyst ranges from 1 to 0.001 to 1 to 0.1, such that the molar ratio of the precursor accounts for 9.1% to 16.66% of the aerogel solution, and the organic solvent is Mohr. The specific content accounts for 83.33% to 90.60% of the aerogel solution, and the molar ratio of the acid catalyst accounts for 0.003% to 0.3% of the aerogel solution; B. one of the aerogel solutions is added The alkali catalyst aqueous solution is subjected to a condensation reaction to form an aqueous aerogel solution, and the alkali catalyst aqueous solution is contacted by a base. The medium is configured with an aqueous solution, and the molar ratio of the alkali catalyst to the aqueous solution is in the range of 0.003 to 16 to 0.2 to 180, and the molar ratio of the precursor in the aerogel aqueous solution after the condensation reaction The content accounts for 0.32% to 7.07% of the aqueous solution of the aerogel, and the molar ratio of the ethanol accounts for 1.61% to 21.20% of the aqueous solution of the aerogel, and the molar ratio of the aqueous solution contains the aqueous solution of the aerogel. 70.67%至98.02%, the molar ratio of the base catalyst is 0.05% to 1.06% in the aqueous solution of the aerogel; C. impregnating a wooden material with the aqueous solution of aerogel, resulting from gelation An aerogel coating the wood material; D. drying the wood material to form a fireproof material.
上述步驟A之水解時間為10分鐘至300分鐘，該前驅物和該酸觸媒的莫耳比含量範圍為1比0.001時，該水解時間為300分鐘，該前驅物和該酸觸媒的莫耳比含量範圍為1比0.1時，該水解時間為10分鐘。The hydrolysis time of the above step A is from 10 minutes to 300 minutes, and the molar ratio of the precursor and the acid catalyst ranges from 1 to 0.001, the hydrolysis time is 300 minutes, and the precursor and the acid catalyst are not When the ear ratio content is in the range of 1 to 0.1, the hydrolysis time is 10 minutes.
上述水及該乙醇之有機溶劑係選自：C1-C5醇類之一或其組合。The water and the organic solvent of the ethanol are selected from one or a combination of C1-C5 alcohols.
上述酸觸媒係選自：一鹽酸、一硫酸或一苯磺酸之強酸，該鹼觸媒係選自：一NH4 OH、一NaOH或一KOH之鹼。The above acid catalyst is selected from the group consisting of: a strong acid of monohydrochloric acid, monosulfuric acid or monobenzenesulfonic acid, and the base catalyst is selected from the group consisting of: a NH 4 OH, a NaOH or a KOH base.
上述步驟B之縮合反應時間為10分鐘至72小時，該鹼觸媒和該酸觸媒的莫耳比含量範圍為1比1時，該縮合反應時間為72小時，該鹼觸媒和該酸觸媒的莫耳比含量範圍為3比1時，該縮合反應時間為10分鐘。The condensation reaction time in the above step B is from 10 minutes to 72 hours, and the molar ratio of the base catalyst and the acid catalyst is in the range of 1 to 1, the condensation reaction time is 72 hours, and the alkali catalyst and the acid are used. When the molar ratio of the catalyst is in the range of 3 to 1, the condensation reaction time is 10 minutes.
上述木質材料係為一木屑、一拋削木片、一拋削木材顆粒、一廢木塊、一木材下腳料其中之一或其組合。The wood material is one of wood chips, one throwing wood chip, one throwing wood grain, one waste wood block, one wood scrap, or a combination thereof.
上述步驟C之凝膠化時間為3分鐘至1100分鐘，該鹼觸媒和該酸觸媒的莫耳比含量為1比1時，該凝膠化時間為1100分鐘，該鹼觸媒和該酸觸媒的莫耳比含量為3比1時，該凝膠化時間為3分鐘。The gelation time of the above step C is from 3 minutes to 1100 minutes, and when the molar ratio of the alkali catalyst and the acid catalyst is 1:1, the gelation time is 1,100 minutes, the alkali catalyst and the alkali catalyst When the molar ratio of the acid catalyst was 3 to 1, the gelation time was 3 minutes.
上述步驟D之乾燥溫度係為25℃至105℃，乾燥時間則最少為30分鐘。The drying temperature in the above step D is from 25 ° C to 105 ° C, and the drying time is at least 30 minutes.
本發明亦可為一種木質材料結合氣凝膠之防火材，係以上述木質材料結合氣凝膠之防火材製造方法所製造而成。The invention may also be a fireproof material of a wood material combined with an aerogel, which is manufactured by the above method for manufacturing a wood material combined with an aerogel fireproof material.
上述防火材中所含之該氣凝膠之重量比含量以0.5wt%至10wt%為最佳。The weight ratio of the aerogel contained in the fireproof material is preferably from 0.5% by weight to 10% by weight.
根據上述技術特徵係具有下列之優點：According to the above technical features, the following advantages are obtained:
1.主要係以回收之木屑為主，故製造成本相當低廉，適合於大量製造及使用。1. Mainly based on recycled wood chips, the manufacturing cost is quite low, and it is suitable for mass production and use.
2.藉由結合多孔性氣凝膠材料的高隔熱特性，以及回收木屑的力學性質等優異特性，並能在一般條件(常溫常壓)下大量製造成防火材，於燃燒中無釋放有毒氣體，安全穩定性佳，可應用於室內裝潢用系統櫃、隔間木材之防火、隔熱，或是建築、工業廠房用之耐火隔熱材上等用途。2. By combining the high heat insulating properties of the porous aerogel material and the mechanical properties of the recovered wood chips, and capable of mass-producing fireproof materials under normal conditions (normal temperature and normal pressure), no release is toxic during combustion. Gas, safety and stability, can be applied to system cabinets for interior decoration, fireproofing and heat insulation of partition wood, or fire-resistant insulation materials for construction and industrial plants.
3.藉由調整酸觸媒濃度，藉以可調整水解反應的時間，以及藉由調整鹼觸媒含量，藉以可調整縮合反應時間，以供視不同需求而降低製造時間。3. By adjusting the acid catalyst concentration, the time of the hydrolysis reaction can be adjusted, and by adjusting the alkali catalyst content, the condensation reaction time can be adjusted to reduce the manufacturing time depending on the demand.
4.氣凝膠溶膠之乾燥程序係於常溫常壓下進行，或利用105℃進行氣凝膠溶膠快速汽化乾燥程序，藉以改善傳統氣凝膠體系之二氧化碳超臨界乾燥程序製成防火材之缺點，可增加回收木屑在防火或阻熱上的機能。4. The aerogel sol drying process is carried out under normal temperature and pressure, or the aerogel sol rapid vaporization drying process is carried out at 105 ° C, thereby improving the disadvantages of the conventional aerogel system carbon dioxide supercritical drying process to produce fireproof materials. It can increase the function of recycling wood chips on fire or heat resistance.
5.以含浸加工方式使，所製造之氣凝膠溶液與回收木屑結合，使該木屑孔洞中以及木屑表面形成氣凝膠保護膜連續結構，以達到結合力強，不易脫落之功效。5. In the impregnation processing method, the manufactured aerogel solution is combined with the recovered wood chips to form a continuous structure of the aerogel protective film in the wood chip hole and the surface of the wood chip, so as to achieve the effect of strong bonding force and not easy to fall off.
6.藉由調整氣凝膠溶液中水與乙醇之含量，可調整該防火材中所含氣凝膠的體積百分比含量，於氣凝膠水溶液中之前驅物的莫耳比含量占1.4%以上時，所製成之防火材即可達到隔熱及防火效果，使該防火材能夠應用在綠建築之防火、隔熱使用。6. By adjusting the content of water and ethanol in the aerogel solution, the volume percentage of the aerogel contained in the fireproof material can be adjusted, and the molar ratio of the precursor in the aerogel aqueous solution accounts for 1.4% or more. When the fireproof material is made, the heat insulation and fireproof effect can be achieved, and the fireproof material can be applied to the fireproof and heat insulation of the green building.
本發明係為一種木質材料結合氣凝膠之防火材製造方法，請參閱第一圖所示，本發明實施例係包括有下列步驟：The invention relates to a method for manufacturing a fireproof material of a wood material combined with an aerogel. Referring to the first figure, the embodiment of the invention comprises the following steps:
A.於一前驅物與一有機溶劑之混合溶液中加入一酸觸媒，使其產生水解反應而成為一氣凝膠溶液。本實施例主要提供一烷氧化矽類或一正矽酸甲酯之前驅物，與以水及乙醇混合而成之有機溶劑，該有機溶劑中之水及乙醇的莫耳比(mol%)含量範圍係為10比1至120比8。將該前驅物與該有機溶劑充分進行攪拌混合成為一混合溶液。又該前驅物與該有機溶劑中水的莫耳比含量範圍係高於1比4，使該前驅物可加速水解反應。亦即該前驅物的莫耳比含量係占該混合溶液中的9%至16%(本實施例係以1莫耳計算)，該有機溶劑的莫耳比含量係占該混合溶液中的84%至91%(本實施例係以5至10莫耳計算)。A. An acid catalyst is added to a mixed solution of a precursor and an organic solvent to cause a hydrolysis reaction to become an aerogel solution. This embodiment mainly provides an alkoxylated cerium oxide or a methyl decanoate precursor, an organic solvent mixed with water and ethanol, and a molar ratio (mol%) of water and ethanol in the organic solvent. The range is 10 to 1 to 120 to 8. The precursor and the organic solvent are thoroughly stirred and mixed to form a mixed solution. Further, the molar ratio of the precursor to the water in the organic solvent is in a range of more than 1 to 4, so that the precursor accelerates the hydrolysis reaction. That is, the Mohr ratio of the precursor accounts for 9% to 16% of the mixed solution (calculated in this example at 1 mol), and the molar ratio of the organic solvent accounts for 84% of the mixed solution. % to 91% (this embodiment is calculated from 5 to 10 moles).
然後於該混合溶液中添加一酸觸媒，使其成為一氣凝膠溶液，該前驅物與該酸觸媒的莫耳比含量範圍係由1比0.001至1比0.1，當該前驅物和該酸觸媒的莫耳比含量範圍係為1比0.001時，其水解時間約300分鐘。當該前驅物和該酸觸媒的莫耳比含量範圍係為1比0.1時，其水解時間約10分鐘，該酸觸媒含量將會影響水解時間。又該前驅物的莫耳比含量係占該氣凝膠溶液中的9.1%至16.66%(本實施例係以1莫耳計算)，該有機溶劑的莫耳比含量係占該氣凝膠溶液中的83.33%至90.60%(本實施例係以5至10莫耳計算)，該酸觸媒的莫耳比含量係占該氣凝膠溶液中的0.003%至0.3%(本實施例係以0.001至0.1莫耳計算)。Then, an acid catalyst is added to the mixed solution to make it an aerogel solution, and the molar ratio of the precursor to the acid catalyst ranges from 1 to 0.001 to 1 to 0.1, when the precursor and the precursor When the molar ratio of the acid catalyst is in the range of 1 to 0.001, the hydrolysis time is about 300 minutes. When the molar ratio of the precursor and the acid catalyst is in the range of 1 to 0.1, the hydrolysis time is about 10 minutes, and the acid catalyst content will affect the hydrolysis time. Further, the Mohr ratio of the precursor accounts for 9.1% to 16.66% of the aerogel solution (calculated in this example at 1 mol), and the molar ratio of the organic solvent accounts for the aerogel solution. 83.33% to 90.60% (calculated in this example is 5 to 10 moles), the molar ratio of the acid catalyst is 0.003% to 0.3% in the aerogel solution (this embodiment is 0.001 to 0.1 m calculated).
上述水解反應係在室溫條件下攪拌進行。又該水解反應時間以30分鐘至60分鐘為最佳，該水解反應時間係隨著該酸觸媒的莫耳百分比含量增加而縮短。水分子於水解反應過程中會與該前驅物之烷氧化矽類或該正矽酸甲酯反應轉換成乙醇，使體系形成該氣凝膠溶液。其中，該酸觸媒係選自：一鹽酸、一硫酸或一苯磺酸之強酸，而該水及乙醇之有機溶劑係選自：C1-C5醇類之一或其組合。The above hydrolysis reaction is carried out under stirring at room temperature. Further, the hydrolysis reaction time is preferably from 30 minutes to 60 minutes, and the hydrolysis reaction time is shortened as the molar percentage of the acid catalyst increases. During the hydrolysis reaction, the water molecules are converted into ethanol by reacting with the alkoxide or the methyl orthoformate of the precursor to form the aerogel solution. Wherein, the acid catalyst is selected from the group consisting of: a strong acid of monohydrochloric acid, monosulfuric acid or monobenzenesulfonic acid, and the organic solvent of the water and ethanol is selected from one of: C1-C5 alcohols or a combination thereof.
B.於該氣凝膠溶液中加入一鹼觸媒水溶液，使其產生縮合反應而形成一氣凝膠水溶液。再提供一鹼觸媒與一水溶液配置而成之一鹼觸媒水溶液，該鹼觸媒與該水溶液的莫耳比含量範圍係為0.003比16至0.2比180，該鹼觸媒水溶液係加入至該氣凝膠溶液中，使其產生一縮合反應，藉以形成一氣凝膠水溶液。該鹼觸媒係選自：NH4 OH、NaOH或KOH等鹼，而配置之水溶液係為純水、過濾水、二次水之一或其組合。該鹼觸媒含量將會影響縮合反應時間，當該鹼觸媒和該酸觸媒的莫耳比含量範圍為1比1時，縮合反應時間約72小時。當該鹼觸媒和該酸觸媒的莫耳比含量範圍為3比1時，縮合反應時間約10分鐘。該縮合反應時間係隨著該鹼觸媒的莫耳比含量增加而縮短。其中，經縮合反應後之整體氣凝膠水溶液中，該前驅物的莫耳比含量係占該氣凝膠水溶液的0.32%至7.07%(本實施例係以1莫耳計算)，該乙醇的莫耳比含量係占該氣凝膠水溶液的1.61%至21.20%(本實施例係以3至5莫耳計算)，而該水溶液的莫耳比含量係占該氣凝膠水溶液的70.67%至98.02% (本實施例係以10至305莫耳計算)，該鹼觸媒的莫耳比含量係占該氣凝膠水溶液中的0.05%至1.06%(本實施例係以0.0015至0.15莫耳計算)。B. Adding an alkali catalyst aqueous solution to the aerogel solution to cause a condensation reaction to form an aerogel aqueous solution. Further, an alkali catalyst aqueous solution is prepared by dissolving a base catalyst and an aqueous solution, and the molar ratio of the alkali catalyst to the aqueous solution is 0.003 to 16 to 0.2 to 180, and the alkali catalyst aqueous solution is added to The aerogel solution is subjected to a condensation reaction to form an aqueous aerogel solution. The base catalyst is selected from the group consisting of a base such as NH 4 OH, NaOH or KOH, and the aqueous solution is one of pure water, filtered water, secondary water or a combination thereof. The base catalyst content will affect the condensation reaction time. When the molar ratio of the base catalyst and the acid catalyst is in the range of 1 to 1, the condensation reaction time is about 72 hours. When the molar ratio of the base catalyst and the acid catalyst is in the range of 3 to 1, the condensation reaction time is about 10 minutes. The condensation reaction time is shortened as the molar ratio of the base catalyst increases. Wherein, in the aqueous aerogel aqueous solution after the condensation reaction, the molar ratio of the precursor is from 0.32% to 7.07% of the aqueous aerogel solution (calculated in this example at 1 mol), the ethanol The molar ratio is from 1.61% to 21.20% of the aqueous solution of the aerogel (calculated in this example at 3 to 5 moles), and the molar ratio of the aqueous solution is 70.67% of the aqueous solution of the aerogel to 98.02% (calculated in this example at 10 to 305 moles), the base catalyst has a molar ratio of 0.05% to 1.06% in the aqueous aerogel solution (this embodiment is 0.0015 to 0.15 moles). Calculation).
C.將一木質材料含浸於該氣凝膠水溶液，經凝膠化而產生一氣凝膠包覆該木質材料。將該木質材料予以含浸至該氣凝膠水溶液中，使該氣凝膠水溶液可以充分滲入該木質材料中。該木質材料以回收之木屑為最佳，除了可以達到最低廉之製造成本外，又該木質材料除了使用回收之木屑外，亦可使用回收拋削木片、回收拋削木材顆粒、回收廢木塊或木材下腳料其中之一或其組合所製造而成。當該鹼觸媒和該酸觸媒的莫耳比含量為1比1時，其凝膠化時間約1100分鐘；而該鹼觸媒和該酸觸媒的莫耳比含量為3比1時，則凝膠化時間縮短至約3分鐘，藉以可控制該木質材料含浸之加工製程時間。又除了透過含浸加工方式外，亦可以連續輸送多道噴灑方式，藉以使該氣凝膠充分滲入該木質材料中。C. Impregnating a wood material into the aerogel aqueous solution, gelling to produce an aerogel coating the wood material. The wood material is impregnated into the aerogel aqueous solution so that the aerogel aqueous solution can sufficiently penetrate into the wood material. The wood material is optimized for the recovered wood chips, in addition to the lowest manufacturing cost, in addition to the recycled wood chips, the wood material can also be used for recycling and cutting wood chips, recycling and throwing wood particles, and recycling waste wood blocks. Or one of or a combination of wood scraps. When the molar ratio of the base catalyst and the acid catalyst is 1 to 1, the gelation time is about 1100 minutes; and the molar ratio of the alkali catalyst and the acid catalyst is 3 to 1. The gelation time is shortened to about 3 minutes, thereby controlling the processing time of the impregnation of the wood material. In addition to the impregnation processing method, a plurality of spray methods can be continuously conveyed, so that the aerogel can fully penetrate into the wood material.
D.使該木質材料乾燥後成型為一防火材。將上述已結合有氣凝膠水溶液之木質材料，於常溫(25℃)及常壓下，可再經由一上膠、一壓縮成型及一乾燥定型等乾燥程序，使其得以成型為一結合有該木質材料及一氣凝膠之防火材。又或於105℃下，進行氣凝膠溶膠快速汽化乾燥程序，藉以改善傳統氣凝膠體系之二氧化碳超臨界乾燥程序製成防火材之缺點，可增加木質材料在防火或阻熱上的機能。在本發明中，由於傳統氣凝膠溶液中，因含有大量的乙醇(酒精)分子，故其在步驟D之乾燥製程期間會形成乙醇蒸氣，當乾燥環境中乙醇蒸氣達氣爆臨界值以上，對於回收之木屑結合氣凝膠所製成之防火材製程的工安有極大的危險性。因此本發明針對回收木屑及氣凝膠結合之防火材所需的氣凝膠溶液製造條件進行改良，藉以可減少製程工安問題。D. The wood material is dried to form a fireproof material. The above-mentioned wood material combined with the aerogel aqueous solution can be formed into a combination by a drying process such as a gluing, a compression molding and a drying setting at normal temperature (25 ° C) and normal pressure. The wood material and an aerogel fireproof material. Or at 105 ° C, the aerogel sol rapid vaporization drying process, in order to improve the conventional aerogel system carbon dioxide supercritical drying process to make fire retardant defects, can increase the performance of wood materials in fire or heat resistance. In the present invention, since the conventional aerogel solution contains a large amount of ethanol (alcohol) molecules, it will form an ethanol vapor during the drying process of the step D, and when the ethanol vapor reaches a critical value of the gas explosion in a dry environment, There is a great danger to the safety of the fireproofing process made of recycled wood chips combined with aerogels. Therefore, the present invention is directed to improving the manufacturing conditions of the aerogel solution required for recovering wood chips and aerogel combined fireproof materials, thereby reducing the problem of process safety.
該步驟D之乾燥條件係為於室溫下進行自然乾燥，或在攝氏80℃至105℃之條件下進行乾燥，如在105℃條件下進行快速攪拌乾燥30分鐘後，即可獲得該防火材，從而提高產品良率。利用該氣凝膠在該木質材料之內部氣腔中形成穩定的一氣凝膠膜，藉以可阻絕該木質材料中之木材纖維素及木質素分子在火焰中快速燃燒。又以含浸加工方式使所製造之氣凝膠水溶液與該回收木屑結合後，於該木屑孔洞中形成氣凝膠保護膜連續結構，可達到結合力強，不易脫落之效果。藉以利用上述製程可以供大量生產且進行連續式工業化製程，進一步可達到降低製造成本之功效。另請參閱附件一所示，其中相片(a)係為回收之木屑，而相片(b)則為本發明以木質材料結合氣凝膠所製成之防火材之實物。The drying condition of the step D is natural drying at room temperature, or drying at 80 ° C to 105 ° C, such as rapid drying and drying at 105 ° C for 30 minutes, the fireproof material can be obtained. , thereby improving product yield. The aerogel is used to form a stable aerogel film in the inner air cavity of the wood material, thereby preventing the wood cellulose and the lignin molecules in the wood material from rapidly burning in the flame. Further, by combining the produced aerogel aqueous solution with the recovered wood chips by an impregnation method, a continuous structure of the aerogel protective film is formed in the wood chip pores, and the bonding force is strong and the peeling effect is not obtained. By utilizing the above process, it is possible to mass-produce and carry out a continuous industrial process, and further reduce the manufacturing cost. Please also refer to Appendix I, where photo (a) is recycled wood chips, and photo (b) is the actual fireproof material made of wood material combined with aerogel.
又前述步驟C之氣凝膠水溶液充分滲入於回收之木屑中，使該回收之木屑中吸附氣凝膠於其內部之孔洞中及木屑之表面。因為原本回收木屑為一擁有大量孔洞的網狀結構，當含浸氣凝膠水溶液後，該氣凝膠水溶液在回收木屑原本的孔洞中凝膠化，當乾燥後氣凝膠也形成擁有大量微孔洞的網狀結構，因此氣凝膠將在回收木屑原本的孔洞中，以及其表面形成多孔性的氣凝膠多孔網狀結構所形成的保護膜，請配合參閱第二圖所示，相片(a)為原回收木屑之外觀照片，相片(b)、(c)及(d)為回收木屑結合氣凝膠改質表面之微觀照片。由照片中可證明該氣凝膠充填於回收木屑之纖維間空隙，並於回收木屑表面形成氣凝膠的一保護膜。其中，前述含浸方式尚可依含浸氣凝膠水溶液中該烷氧化矽類或該正矽酸甲酯含量的多寡，可以製造成不同氣凝膠含量披覆的防火材，亦即低含量之該烷氧化矽類或該正矽酸甲酯的莫耳比含量於含浸該回收木屑，係表示該回收木屑局部受到該氣凝膠保護，除可保留回收木屑的原有外觀及回收木屑的特性外，還外加氣凝膠的高隔熱性與耐火性質，故可應用於綠建築的一般隔熱建材或者汽車用之隔熱材。相對的，高含量之該烷氧化矽類或該正矽酸甲酯的莫耳比含量於含浸該回收木屑，係可使該回收木屑完全受到該氣凝膠保護，可提供較為高級的隔熱性與耐火性質，因此可應用於建築或工業廠房用之耐火隔熱材上。又調整氣凝膠溶液中水與乙醇含量，可藉以調整該防火材中所含該氣凝膠的體積百分比含量，例如氣凝膠水溶液中該前驅物的莫耳比含量占1.4%以上時，所製成之防火材即可達到隔熱及防火效果。Further, the aerogel aqueous solution of the above step C is sufficiently infiltrated into the recovered wood chips, so that the recovered wood chips adsorb the aerogel in the pores inside the surface and the surface of the wood chips. Because the original recovered wood chips is a network structure having a large number of holes, the aqueous aerogel solution gels in the original holes of the recovered wood chips after being impregnated with the aqueous solution of the aerogel, and the aerogel also forms a large number of micropores when dried. The network structure of the hole, so the aerogel will be in the original hole of the recovered wood chip, and the protective film formed on the surface of the porous aerogel porous mesh structure, please refer to the photo shown in the second figure ( a) Photographs of the appearance of the original recovered wood chips, and photographs (b), (c) and (d) are microscopic photographs of the recovered surface of the recycled wood chips combined with the aerogel. It can be confirmed from the photograph that the aerogel is filled in the interfiber space of the recovered wood chips, and a protective film for forming an aerogel on the surface of the recovered wood chips is formed. Wherein, the foregoing impregnation method can still be made into a fireproof material coated with different aerogel content according to the content of the alkoxyus oxide or the methyl orthoformate in the aqueous solution of the impregnated aerogel, that is, the low content The molar ratio of the alkoxylated cerium oxide or the methyl ortho-decanoate to the impregnated wood chips indicates that the recycled wood chips are partially protected by the aerogel, except that the original appearance of the recovered wood chips and the characteristics of the recovered wood chips can be retained. It also has the high heat insulation and fire resistance properties of aerogel, so it can be applied to general insulation building materials for green buildings or heat insulation materials for automobiles. In contrast, the high content of the alkoxylated cerium or the molar ratio of the methyl ortho-methyl phthalate to the impregnated wood chips enables the recovered wood chips to be completely protected by the aerogel, and provides relatively advanced heat insulation. Sexual and refractory properties, so it can be applied to refractory insulation materials for construction or industrial plants. Adjusting the water and ethanol content in the aerogel solution, thereby adjusting the volume percentage of the aerogel contained in the fireproof material, for example, when the molar ratio of the precursor in the aerogel aqueous solution accounts for 1.4% or more, The fireproof material can be used to achieve heat insulation and fireproofing effects.
又該防火材中所含之該氣凝膠之重量比含量係以0.5wt%至10wt%為最佳。該步驟A之該烷氧化矽類或該正矽酸甲酯之該前驅物與該氣凝膠水溶液的莫耳比含量範圍為1：30時，則該回收木屑與該氣凝膠水溶液的體積比範圍為1：0.85至1：1.5。Further, the weight ratio of the aerogel contained in the fireproof material is preferably from 0.5% by weight to 10% by weight. When the molar ratio of the alkoxylated cerium oxide or the precursor of the methyl ortho-nonanoate to the aerogel aqueous solution in the step A is 1:30, the volume of the recovered wood chips and the aerogel aqueous solution is The ratio ranges from 1:0.85 to 1:1.5.
當經過該步驟D乾燥程序後之木質材料中的該木質材料與氣凝膠的體積比在1：1以下時，即能作為一般防焰材使用，藉此節省該氣凝膠的用量以控制製造成本。當該木質材料與氣凝膠的體積比範圍在1：1以上時，除具有優良隔熱效果外，更能達到防火的效果，本發明之回收木屑結合氣凝膠所製成之防火材經燃燒最低含氧量(LOI)測試，該LOI值達50以上，可達一級防火耐焰效果，燃燒中無釋放有毒氣體，安全穩定性佳，故可做為建築用防火隔熱材使用。本發明之回收木屑結合氣凝膠所製成之防火材經綠建材隔熱係數(k)測試，該k值達0.12W/m‧k，比一般木材板材以及木塑板低，具有優異的隔熱效果。該燃燒最低含氧量(LOI)以及綠建材隔熱係數(k)測試數據如下列表一所示。又實物經燃燒試驗之相片如附件二所示，其中相片(a)係為燃燒前之防火材實物相片，而相片(b)則為燃燒後之防火材實物相片。When the volume ratio of the wood material to the aerogel in the wood material after the drying process of the step D is below 1:1, it can be used as a general flame resistant material, thereby saving the amount of the aerogel to control manufacturing cost. When the volume ratio of the wood material to the aerogel is above 1:1, in addition to having an excellent heat insulating effect, the fireproof effect can be achieved, and the fireproof material prepared by the recycled wood chips combined with the aerogel of the present invention is The minimum oxygen content (LOI) test for burning, the LOI value of 50 or more, up to the first stage fire and flame resistance effect, no toxic gas released during combustion, good safety and stability, so it can be used as fireproof and heat insulation material for construction. The fireproof material prepared by the recycled wood chips combined with the aerogel of the invention is tested by the heat insulation coefficient (k) of the green building material, and the k value is 0.12 W/m‧k, which is lower than the general wood board and the wood plastic board, and has excellent performance. Insulation effect. The minimum oxygen content (LOI) of combustion and the thermal insulation coefficient (k) test data of green building materials are shown in the following table 1. Photographs of the actual burning test are shown in Annex 2. Photo (a) is a photo of the fire-retardant material before burning, and photo (b) is a photo of the fire-retardant material after burning.
表一：
本發明亦可為一種木質材料結合氣凝膠之防火材，係依照上述製造方法所製造而成。該防火材中係包含有一回收木屑及一氣凝膠，該氣凝膠與該回收木屑結合形成氣凝膠保護膜結構。該回收木屑與該氣凝膠的重量比範圍在1：1以下時，則具有防焰的效果(LOI＞36)，由於該防火材之防火及防焰效果，係隨著該氣凝膠的重量比增加而提高。因此就能節省氣凝膠的使用量，並兼具隔熱及低成本的功效。The invention may also be a fireproof material of a wood material combined with an aerogel, which is manufactured according to the above manufacturing method. The fireproof material comprises a recycled wood chip and an aerogel, and the aerogel is combined with the recycled wood chip to form an aerogel protective film structure. When the weight ratio of the recycled wood chips to the aerogel is below 1:1, the flameproof effect (LOI>36) is obtained, and the fireproofing and flameproofing effect of the fireproofing material is followed by the aerogel The weight ratio increases and increases. Therefore, the amount of aerogel used can be saved, and both heat insulation and low cost can be achieved.
本發明係結合具多孔性之氣凝膠材料的高隔熱特性以及回收木屑的特性，藉以製成以回收木屑結合氣凝膠之防火材，並且能大量製造，相當具有產業利用性。此外，本發明中藉由調整該酸觸媒含量，以調整該水解反應的時間，及藉由調整該氣凝膠溶液中該鹼觸媒含量，以調整該縮合反應形成凝膠化的時間，以控制該回收木屑含浸加工製程時間。再者，本發明中該氣凝膠可滲入該回收木屑中，並於該木屑孔洞中以及木屑表面形成氣凝膠的保護膜，並使氣凝膠不易脫落。而調整所含之該回收木屑與該氣凝膠的體積比範圍大於1：1以上時，即具有優良的防火效果，使本發明中該回收木屑結合氣凝膠，藉以能作為建築用隔熱、防火材使用。The present invention combines the high heat insulating properties of a porous aerogel material and the characteristics of wood chips to be recovered, thereby producing a fireproof material for recovering wood chips and aerogel, and can be mass-produced, and is quite industrially usable. In addition, in the present invention, by adjusting the acid catalyst content, the time of the hydrolysis reaction is adjusted, and by adjusting the alkali catalyst content in the aerogel solution, the condensation reaction is adjusted to form a gelation time. In order to control the processing time of the recycled wood chips impregnation process. Furthermore, in the present invention, the aerogel can be infiltrated into the recovered wood chips, and a protective film of the aerogel is formed in the wood chip holes and on the surface of the wood chips, and the aerogel is not easily peeled off. When the volume ratio of the recovered wood chips and the aerogel contained in the adjustment is greater than 1:1, the fireproof effect is excellent, so that the recycled wood chips in the present invention are combined with aerogel, thereby being used as insulation for construction. , fireproof materials are used.
惟，以上所述僅為本發明其中之二實施例，當不能以此限定本發明之申請專利保護範圍，舉凡依本發明之申請專利範圍及說明書內容所作之簡單的等效變化與替換，皆應仍屬於本發明申請專利範圍所涵蓋保護之範圍內。However, the above description is only two of the embodiments of the present invention, and the scope of the patent application and the scope of the description of the present invention are not limited thereto. It is still within the scope of the protection covered by the scope of the invention.
無no
[第一圖]係為本發明之步驟流程圖。[First figure] is a flow chart of the steps of the present invention.
[第二圖]係為本發明實施例中之回收木屑於製造前及製造後與氣凝膠結合成為一防火材之電子顯微鏡照片。[Second image] is an electron micrograph of the fire-retardant material which is combined with the aerogel before and after manufacture in the embodiment of the present invention.
[表一]係為本發明實施例中所製成之防火材進行燃燒最低含氧量(LOI)測試之數據表。[Table 1] is a data sheet for performing a combustion minimum oxygen content (LOI) test for the fireproof material produced in the examples of the present invention.
[附件一]係為本發明實施例中所使用之回收木屑及其製造成為防火材之實物相片。[Attachment 1] is a physical photograph of recycled wood chips used in the embodiments of the present invention and their manufacture as fireproof materials.
[附件二]係為本發明實施例中所製成之防火材進行燃燒前、後對比之外觀相片。[Attachment 2] is an appearance photograph of the fireproof material prepared in the examples of the present invention before and after combustion.
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