Ham reçineden AlCl3 eşliğinde doğal terpen-rosin fenolik reçinelerin sentezi ve karakterizasyonu: Sıcaklığın etkisi
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Dosyalar
Tarih
2023
Yazarlar
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Yayıncı
Bursa Teknik Üniversitesi, Lisansüstü Eğitim Enstitüsü
Erişim Hakkı
info:eu-repo/semantics/openAccess
Özet
Reçine, başta kimya, kağıt, kozmetik, boya ve ilaç sektörü olmak üzere birçok farklı sektörde kullanılan oldukça değerli bir odun dışı orman ürünüdür. Türkiye, reçine üretimine elverişli kızılçam ormanlarına sahip olmasına rağmen yeteri kadar reçine üretimi yapılamamakta ve üretilen reçine piyasaya türevlendirilmeden ham olarak sunulmaktadır. Reçine ihtiyacı tamamen ithalat yoluyla karşılanmaktadır. Gelişmiş birçok ülke reçineyi endüstriyel ürünlere dönüştürerek ekonomik olarak kazanç sağlamaktadır. Reçinenin yapısında bulunan terpenler yenilenebilir biyo-esaslı malzemeler için önemli bir potansiyel oluşturmaktadır. Özellikle kimya sektöründe birçok reaksiyonda başlatıcı olarak kullanılmaktadır. Günümüzde kullanılan sentetik reçinelerin çevreye verdiği zararlı etkileri ve kullanımına getirilen kısıtlamalar sebebiyle biyobozunur malzemelere ilgi ve talep giderek artmaktadır. Petrokimyasal ürünler yerine reçine gibi doğal ve çevreye uyumlu ürünler kullanılması hem çevreye hem de insan sağlığına olumlu yönde katkılar sağlayacaktır. Bu çalışma kapsamında, Balıkesir-Edremit'teki kızılçam ağaçlarının köklerinden ekstraksiyon yöntemiyle elde edilen ham reçine (CWR) ve damıtma ürünü terebentin kullanılarak reçinenin bir türevi olan terpen-rosin fenolik reçine sentezi gerçekleştirilmiştir. Farklı beş sıcaklıkta (40 °C, 50 °C, 60 °C, 70 °C ve 80 °C) üretilen deney örnekleri üzerinde sıcaklık etkisi incelenmiştir. Üretim safhasına geçmeden önce ham reçine distilasyon ile terebentin ve kolofana ayrılmış ve gaz kromotografi - kütle spektroskopisi (GC-MS) cihazı ile karakterize edilmiştir. GC-MS analiz sonuçlarına bakıldığında, terebentin yapısında bulunan 4 baskın bileşen sırasıyla α-pinen (%71,60), limonen (%9,11), kamfen (%8,3) ve β-pinen (%3,14) olarak tespit edilmiştir. Kolofanın yapısında ise en çok bulunan dört baskın bileşen sırasıyla dehidroabietik asit (%26,25), abietik asit (%10,06), podokarpik asit (%5,4) ve dihidroisopimarik asit (%5,01) olarak bulunmuştur. Terpen-rosin fenolik reçine örneklerinde, FTIR (Fourier-dönünüşümlü kızılötesi spektroskopisi) analizi, asit sayısı, sabunlaşma sayısı, yumuşama noktası ve renk tayini yapılmıştır. Analizler sonucunda; asit sayısı 104,11 ile 90,79 arasında; sabunlaşma sayısı 141,05 ile 105,07 arasında bulunmuştur. En yüksek asit sayısı 50 °C'de üretilen örnekte bulunurken en düşük asit sayısı 80 °C'de üretilen örnekte bulunmuştur. En yüksek sabunlaşma sayısı 50 °C'de üretilen örnekte bulunurken en düşük asit sayısı 60 °C'de üretilen örnekte bulunmuştur. Yumuşama noktası 70,80 ile 79,00 °C arasında bulunmuştur. En yüksek yumuşama noktasının 40 °C'de üretilen örneğe ait olduğu görülmüştür. Örneklerin rengi koyu-kahverengi-amber olarak tespit edilmiştir. En yüksek verim ise %82,16 ile 60 °C'de üretilen örnekte bulunurken en düşük verim 50 °C'de hazırlanan örnekte %79,90 olarak bulunmuştur. FTIR analizinde, kuvvetli bir şekilde kendini gösteren C-H ve karbonil (C=O) gerilme pikleri ile C=C gerilme titreşim pikleri gözlemlenmiştir. Karakteristik fenol bantları gözlemlenmiştir.
Resin is a very valuable non-wood forest product used in many different sectors, especially in the chemistry, paper, cosmetics, paint and pharmaceutical industries. Although Turkey has red pine forests suitable for resin production, enough resin cannot be produced and the produced resin is presented to the market as raw without derivatization. The need for resin is completely met through imports. Many developed countries make economic gains by converting resin into industrial products. Terpenes in the structure of the resin represent an important potential for renewable bio-based materials. It is used as an initiator in many reactions, especially in the chemical industry. Due to the harmful effects of synthetic resins used today and the restrictions on their use, interest and demand for biodegradable materials is increasing. Using natural and environmentally compatible products such as resin instead of petrochemical products will contribute positively to both the environment and human health. In this study, terpene-rosin phenolic resin, a derivative of the resin, was synthesized by using raw resin (CWR) extracted from the roots of red pine trees in Balıkesir-Edremit, and turpentine, a distillation product. The effect of temperature on test samples produced at five different temperatures (40 ⁰C, 50 ⁰C, 60 ⁰C, 70 ⁰C and 80 ⁰C) was investigated. Before proceeding to the production part, the crude wood rosin was separated into turpentine and rosin by distillation and characterized by gas chromatography (GC-MS) and mass spectroscopy device. As a result of GC-MS analysis, the 4 dominant components in the turpentine structure were determined as alpha-Pinene (71.60%), limonene (9.11%), camphene (8.3%) and betapinene (3.14%). In the structure of rosin, the four most dominant components were dehydroacetic acid (26.25%), abietic acid (10.06%), podocarpic acid (5.4%) and dihydroisopimaric acid (5.01%). FTIR (Fourier-transform infrared spectroscopy) analysis, acid number, saponification number, softening point and color determination were performed on terpene-rosin phenolic resin samples. As a result of the analysis; acid number between 104.11 and 90.79; the saponification number was found to be between 141.05 and 105.07. The highest acid number was found in the sample produced at 50 °C, while the lowest acid number was found in the sample produced at 80 °C. The highest saponification number was found in the sample given at 50 °C, while the lowest acid number was found in the sample produced at 60 °C. The softening point was found between 70.80 and 79.00 °C. It was observed that the highest softening point belonged to the sample produced at 40 °C. The color of the samples was determined as dark-brown-amber. The highest efficiency was found in the sample produced at 60 °C with 82.16%, while the lowest efficiency was found as 79.90% in the sample produced at 50 °C. In the FTIR analysis, strong C-H and carbonyl (C=O) stretching peaks and C=C stretching vibration peaks were observed. Characteristic phenol bands were observed.
Resin is a very valuable non-wood forest product used in many different sectors, especially in the chemistry, paper, cosmetics, paint and pharmaceutical industries. Although Turkey has red pine forests suitable for resin production, enough resin cannot be produced and the produced resin is presented to the market as raw without derivatization. The need for resin is completely met through imports. Many developed countries make economic gains by converting resin into industrial products. Terpenes in the structure of the resin represent an important potential for renewable bio-based materials. It is used as an initiator in many reactions, especially in the chemical industry. Due to the harmful effects of synthetic resins used today and the restrictions on their use, interest and demand for biodegradable materials is increasing. Using natural and environmentally compatible products such as resin instead of petrochemical products will contribute positively to both the environment and human health. In this study, terpene-rosin phenolic resin, a derivative of the resin, was synthesized by using raw resin (CWR) extracted from the roots of red pine trees in Balıkesir-Edremit, and turpentine, a distillation product. The effect of temperature on test samples produced at five different temperatures (40 ⁰C, 50 ⁰C, 60 ⁰C, 70 ⁰C and 80 ⁰C) was investigated. Before proceeding to the production part, the crude wood rosin was separated into turpentine and rosin by distillation and characterized by gas chromatography (GC-MS) and mass spectroscopy device. As a result of GC-MS analysis, the 4 dominant components in the turpentine structure were determined as alpha-Pinene (71.60%), limonene (9.11%), camphene (8.3%) and betapinene (3.14%). In the structure of rosin, the four most dominant components were dehydroacetic acid (26.25%), abietic acid (10.06%), podocarpic acid (5.4%) and dihydroisopimaric acid (5.01%). FTIR (Fourier-transform infrared spectroscopy) analysis, acid number, saponification number, softening point and color determination were performed on terpene-rosin phenolic resin samples. As a result of the analysis; acid number between 104.11 and 90.79; the saponification number was found to be between 141.05 and 105.07. The highest acid number was found in the sample produced at 50 °C, while the lowest acid number was found in the sample produced at 80 °C. The highest saponification number was found in the sample given at 50 °C, while the lowest acid number was found in the sample produced at 60 °C. The softening point was found between 70.80 and 79.00 °C. It was observed that the highest softening point belonged to the sample produced at 40 °C. The color of the samples was determined as dark-brown-amber. The highest efficiency was found in the sample produced at 60 °C with 82.16%, while the lowest efficiency was found as 79.90% in the sample produced at 50 °C. In the FTIR analysis, strong C-H and carbonyl (C=O) stretching peaks and C=C stretching vibration peaks were observed. Characteristic phenol bands were observed.
